CN111086118B

CN111086118B - Pigment solvent bottle regeneration treatment device and method

Info

Publication number: CN111086118B
Application number: CN201911310115.XA
Authority: CN
Inventors: 肖于才; 张伟; 刘邦坤; 何守琴; 马书民; 熊宁; 宁亮; 高丹
Original assignee: XUANCHENG YABANG CHEMICAL CO Ltd
Current assignee: Anhui Shenlanhua Color Material Co ltd
Priority date: 2019-12-18
Filing date: 2019-12-18
Publication date: 2021-01-01
Anticipated expiration: 2039-12-18
Also published as: CN111086118A

Abstract

The invention relates to a regeneration treatment device and a regeneration treatment method for a pigment solvent bottle, wherein the device comprises a vertical double-barrel stirrer, a kneading machine, a condensing device and a first storage tank which are communicated in sequence; the vertical double-barrel stirrer comprises an outer barrel and a liftable inner barrel, wherein more than one layer of gauze is horizontally arranged in the inner barrel, small holes are uniformly formed in the barrel wall of the inner barrel, the outer barrel is provided with a feeding port and a discharging port, and a vacuum exhaust port is formed in the top of the outer barrel; the kneading machine comprises a feeding port and a discharging port, the feeding port is connected with the discharging port of the vertical double-barrel stirrer, and the discharging port is connected with the condensing device; the top of the first storage tank is provided with a feeding port and a vacuum exhaust port, the bottom of the first storage tank is provided with a discharge port, the feeding port of the first storage tank is connected with condensing equipment, and the discharge port of the first storage tank is connected with the feeding port of the vertical double-barrel stirrer; the vacuum exhaust port of the vertical double-barrel stirrer and the vacuum exhaust port of the storage tank are connected with vacuum pumps. The device recycles the solvent and the coloring resin in the solvent bottle, and realizes the sustainable utilization and development of resources.

Description

Pigment solvent bottle regeneration treatment device and method

Technical Field

The invention relates to the field of recycling of industrial solvent bottles, in particular to a device and a method for regenerating and treating a solvent bottle for pigment.

Background

The phthalocyanine blue pigment is a blue organic pigment with very excellent fastness, and with the rapid development of industrial coatings, printing inks, dyes and pigments, more and more industrial color matching application fields need to be tested and detected, particularly, the phthalocyanine blue is applied to industrial coloring systems such as solvent paints, solvent inks and the like, and the application and detection needs to be matched with a large number of solvent bottles, wherein the solvent bottles comprise glass bottles, plastic bottles, glass beads, zirconium beads, steel balls, synthetic resins, mixed solvents, pigments, fillers, dispersing agents and the like, and the components are extremely complex. Due to the particularity of the resin and the organic solvent, the solvent bottle is usually treated in a landfill incineration mode after detection, so that the solvent bottle and other media can only be used once, the resource waste is great, the cost is high, and the solvent bottle is urgently required to be cleaned and reused in a laboratory.

The resin is mainly artificial synthetic resin, such as alkyd resin, polyester resin, chlorinated polypropylene resin, polyvinyl chloride resin, nitrocotton resin, polyurethane resin and the like; the solvent mainly comprises a mixed solvent composed of aromatic hydrocarbons, lipids, alcohols, ethers, ketones and the like; the pigment mainly comprises organic pigment and inorganic pigment, such as phthalocyanine pigment, titanium pigment, etc.; the filler mainly comprises barium sulfate, calcium carbonate, talcum powder and the like.

At present, a plurality of devices and methods for cleaning solvent bottles exist, and an invention patent with the application number of CN201610556682.3 discloses an automatic high-purity solvent bottle cleaning device. The invention patent with application number CN201610892740.X discloses a cleaning agent bottle with high protection measures, which comprises an arc-shaped base, wherein a heavy object is arranged in an inner cavity of the arc-shaped base, only a solvent bottle base is arranged in the inner cavity, baffles are arranged on two sides of the solvent bottle base, a solvent bottle is connected to the top of the solvent bottle, a shockproof coat and a shockproof sponge are arranged on the outer surface of the solvent bottle, and the solvent bottle is cleaned through a nozzle arranged at the top of the solvent bottle. The invention patent with the application number of CN201610994462.9 discloses an automatic cleaning device for a glass sample bottle, which comprises a solvent bottle, a plunger pump, a pipeline, support legs, a solvent spray head, the sample bottle, a sample bottle wheel disc, a sealing shaft, a speed reduction motor, a bottom plate, a glass cover, a nozzle base and a sealing plug, wherein the sample bottle is reversely buckled in a fixing groove of the wheel disc, the glass cover is used for ensuring sealing, the speed of the plunger pump and the cleaning time are set, the speed regulation motor is started to ensure that the sample bottle is fully contacted with the solvent, the plunger pump is started, the sample bottle is cleaned in a high-pressure cleaning mode, a brush cleaning process is not needed, and different solvents can be exchanged according to different pollutants for cleaning.

Disclosure of Invention

The inventor finds that although batch cleaning dedicated equipment appears in recent years, the technology is still not mature, incomplete and systematic. Some devices can be only used for aqueous cleaning agents, some aqueous sample vials can be cleaned, or some sample vials only containing solvents are cleaned, and the devices are not suitable for colored solvent media with high resin, high filling and high pigment concentration at all, and particularly after phthalocyanine blue color matching detection, the solvent vials need to be stored for a long time, thickened conditions are observed, and then treatment is carried out. Thus, the solvent bottles are of a high consistency, small batch, intermittent, fragile, flammable, explosive type and are difficult to clean. At present, if the medium such as a solvent bottle is required to be reused, manual cleaning or partial recovery is required only when the medium is small in quantity, and in the cleaning process, the mixed solvent in the solvent bottle is too big in taste and is in contact with the medium for a long time, so that the mixed solvent is unfavorable for human health after being inhaled. At present, benzene and lipid solvents are mostly injected in a manual cleaning method, a hairbrush is inserted for manual stirring cleaning or hand-cranking cleaning, the cleaning process consumes time, the solvent volatilization is serious, the working efficiency is extremely low, and the requirement of color matching detection in phthalocyanine pigment application cannot be normally met. The fundamental reason is that no effective method is available for separating, recovering and recycling pigments, solvents, resins, glass bottles and the like at present. If a classification method is adopted, solvent bottles with various resin system purposes are classified and collected, color paste in the bottles is sent to various professional ink and paint manufacturers for treatment, the method is theoretically feasible, but the safety problem in the actual transportation link cannot be guaranteed, a freight carrier cannot carry the color paste, the manufacturers are not willing to treat the test solid waste and the color paste with small relative quantity, and the quality risk after actual treatment is very high because the recovered color paste is carried and can cause unpredictable effect on the product quality of the manufacturers, and importantly, glass bottles and plastic bottles after the color paste is poured cannot be cleaned, so that a laboratory cannot simulate application detection of downstream customers during solvent type application color matching detection. Under the special background, a method for effectively regenerating and treating the solvent bottle is urgently needed by phthalocyanine pigment manufacturers, and the inspection and control of the shipment quality of the phthalocyanine blue pigment are ensured.

The technical problem solved by the invention is as follows: the prior solvent bottle cleaning equipment and method have the following defects: 1. the labor efficiency is low, the transportation is unsafe, and the recycled color paste is risky; 2. the operation environment is severe, and the physical and psychological health is not easy to happen; 3. the pigment, solvent, resin, glass bottle and the like in the solvent bottle for the pigment are not separated, recycled and regenerated by an effective method, so that the resource waste is caused; in addition, the present invention finds, in the process of continuously improving the solvent bottle recycling apparatus: 1. the separation speed of the solvent, the pigment and the resin is slow during low-temperature distillation; 2. the leakage prevention of the equipment during kneading and distillation cannot be solved, so that the flammable and explosive safety level cannot be reduced; 3. the colored resin remaining after distillation cannot be effectively separated from the equipment container; 4. the distilled pigment resin cannot be recycled effectively.

The purpose of the invention is: provided are an efficient, safe, continuously-operable and resource-recyclable solvent bottle recycling device and method for pigments, particularly for industrial match detection test bottles, for example, a device and method for recycling solvent bottles dedicated for phthalocyanine blue match detection.

In order to solve the technical problems, the invention provides a device and a method for regenerating a solvent bottle for pigment.

Specifically, aiming at the defects of the prior art, the invention provides the following technical scheme:

a solvent bottle regenerating device for pigment is characterized by comprising a vertical double-barrel stirrer 1, a kneader 2, a condensing device 3 and a first storage tank 4 which are communicated in sequence;

the vertical double-barrel stirrer comprises an outer barrel 11 and a liftable inner barrel 12, wherein more than one layer of gauze is horizontally arranged in the inner barrel 12, small holes are uniformly formed in the barrel wall of the inner barrel 12, the outer barrel 11 is provided with a first feeding hole 15 and a first discharging hole 16, and a first vacuum exhaust port 17 is formed in the top of the outer barrel 11;

the kneading machine 2 comprises a feeding port and a discharging port, the feeding port is connected with the discharging port of the vertical double-barrel stirrer, and the discharging port is connected with a condensing device;

a second feeding port 40 and a second vacuum exhaust port 41 are arranged at the top of the first storage tank 4, a second discharging port 42 is arranged at the bottom of the first storage tank 4, the second feeding port 40 of the first storage tank 4 is connected with the condensing equipment 3, and the second discharging port 42 of the first storage tank 4 is connected with the first feeding port 15 of the vertical double-barrel stirrer;

the first vacuum exhaust port 17 of the vertical twin-tub agitator and the second vacuum exhaust port 41 of the first storage tank are connected with a vacuum pump 5.

Preferably, the vertical double-barrel stirrer comprises a barrel cover, and a sealing gasket is arranged between the barrel cover and the barrel body.

Preferably, in the regeneration device, a second storage tank 6 is arranged between the vertical twin-tub agitator 1 and the first storage tank 4, the second storage tank 6 includes a feed opening and an upper vent, the feed opening is connected with the first discharge opening 16 of the vertical twin-tub agitator, and the upper vent is connected with the second feed opening 40 of the first storage tank 4.

Preferably, in the above regenerating device, a valve is disposed at a feeding port of the kneader, valves are disposed at a feed port and an upper exhaust port of the second storage tank, and preferably, the upper exhaust port valve of the second storage tank is a three-way ball valve.

Preferably, in the above regeneration apparatus, the feed port, the discharge port, and the vacuum exhaust port of the vertical twin-tub agitator are provided with valves.

Preferably, in the above regenerating apparatus, a discharge port of the kneader and an inlet of the vacuum pump are provided with valves.

Preferably, in the above regeneration apparatus, the feed port, the discharge port, and the vacuum exhaust port of the first storage tank are provided with valves.

Preferably, in the above regeneration apparatus, the vertical twin-tub agitator 1 includes a motor 13, the motor 13 is connected to an agitation shaft 14, the agitation shaft 14 is disposed at the center of the tub, and an end of the agitation shaft 14 is connected to the inner tub 12.

Preferably, in the above regenerating apparatus, the ratio of the inner drum diameter to the outer drum diameter of the vertical twin-drum agitator 1 is 1: (1.2-1.4).

Preferably, in the above regenerating device, the vertical twin-tub agitator 1 has an outer tub volume of 30 to 80L and an inner tub volume of 20 to 40L.

Preferably, in the above regeneration device, the gauze in the inner barrel of the vertical twin-barrel agitator 1 is 5-30 mesh, and the small holes on the barrel wall of the inner barrel are 5-30 mesh.

Preferably, in the above regenerating device, the number of layers of the gauze in the inner barrel is 2 to 5.

Preferably, in the above regenerating apparatus, the kneader is provided with a kneading unit, a transmission unit, a heating unit, an electric control unit, and a temperature control unit.

The invention also provides a regeneration method of the solvent bottle for the pigment, which is characterized by comprising the following steps:

(1) solvent bottle washing process: opening the regeneration device, uniformly placing the solvent bottle upside down on a gauze in an inner barrel of the vertical double-barrel stirrer 1, adding a mixed solvent, and washing the solvent bottle to obtain a mixture of the solvent and the color paste; starting a vacuum pump, pumping the obtained solvent and color paste mixture into a kneader, lifting an inner barrel, and taking out a clean solvent bottle;

(2) kneading and dispersing process: starting a kneader, adding a medicament, uniformly kneading, introducing the mixture obtained in the step (1) into the kneader, setting the temperature of a kneading unit to be 60-80 ℃, performing low-temperature dispersion and flocculation, and distilling to obtain a solvent to enter a first storage tank;

(3) high-temperature kneading process: setting the temperature of a kneading unit in a kneader to be 80-145 ℃, and kneading at high temperature until all the solvent is removed by distillation;

(4) and (3) color master recovery process: and closing the kneading machine, and cooling the materials in the kneading machine to obtain the color master.

Preferably, in the regeneration method, the temperature of the high-temperature kneading process is 100-145 ℃, and preferably 135-145 ℃.

Preferably, in the regeneration method, in the step (2), the mass ratio of the mixture of the solvent and the color paste, which is firstly added into the kneader, to the chemical agent is 25: (1-20).

Preferably, in the regeneration method, the mass ratio of the mixture of the solvent and the color paste in the kneader to the medicament is 25: (1-20), preferably 25: (1-10).

Preferably, in the above recycling method, in the step (1), the mixture of the solvent and the color paste obtained by the vertical twin-tub agitator is pumped into the kneader or the second storage tank.

Preferably, in the above regeneration method, the regeneration method includes any one of the following processes:

firstly pumping the solvent and color paste mixture obtained by the vertical double-barrel stirrer into a kneader, and pumping the excessive solvent and color paste mixture into a second storage tank when the requirement of the kneader is met; in the step (2), closing an upper vent valve of the second storage tank, opening a feed opening valve of the second storage tank and a feed opening valve of the kneader, and pumping the mixture of the solvent and the color paste in the second storage tank into the kneader; or

Pumping all the solvent and color paste mixture obtained by the vertical double-barrel stirrer into a second storage tank; in the step (2), the upper vent valve of the second storage tank is closed, the feed opening valve of the second storage tank and the feed opening valve of the kneader are opened, and the mixture of the solvent and the color paste in the second storage tank is pumped into the kneader.

Preferably, in the regeneration method, the mixed solvent in the step (1) comprises alcohol ether and ester, and the mass ratio of the alcohol ether to the ester is 1 (10-25); preferably, the alcohol ether is one or more selected from propylene glycol methyl ether, ethylene glycol methyl ether, diethylene glycol methyl ether, triethylene glycol methyl ether, ethylene glycol monopropyl ether and diethylene glycol monopropyl ether, and the ester is one or more selected from ethyl acetate, methyl acetate, propyl acetate, butyl acetate, diethylene glycol propyl ether acetate and propylene glycol ethyl ether acetate.

Preferably, in the regeneration method, the addition amount of the mixed solvent is 1/3-2/3 of the volume of the outer barrel of the vertical double-barrel stirrer 1.

Preferably, in the above regeneration method, the washing process in step (1) includes a stirring process, and the stirring speed is 200-500 rpm.

Preferably, in the above regeneration method, the number of repetitions of step (1) is 3 to 5.

Preferably, in the above regeneration method, the washing process in step (1) further comprises the steps of: blowing nitrogen into a vertical double-barrel stirrer to blow off solvent residues.

Preferably, in the above regeneration method, the degree of vacuum of the kneader in the step (2) and the step (3) is set to-0.02 to-0.045 MPa.

Preferably, in the above regeneration method, the time for kneading at a low temperature in step (2) is 15 to 20 min.

Preferably, in the above regeneration method, the pharmaceutical agent in step (2) comprises resin, calcium carbonate, bentonite and magnesium stearate, and the mass ratio is 100: (20-50): (10-30): (20-30); the resin is selected from one or more of PVC paste resin, polyvinyl chloride resin, polyurethane resin and chlorinated polypropylene resin.

Preferably, in the recycling method, the color masterbatch recycling process in step (4) includes the following steps: and (4) closing the kneader, taking out the materials in the kneader when the temperature is reduced to 60-75 ℃, cooling and standing for 72-168 hours to obtain the color master.

Preferably, in the above recycling method, the solvent bottle in the step (1) contains a pigment, a carrier resin and a solvent. The carrier resin is selected from one or more of polyurethane resin, chlorinated polypropylene resin, alkyd resin, polyester resin, PVC paste resin, nitrocotton resin and epoxy resin. The pigment is preferably phthalocyanine blue, and the solvent is selected from toluene, xylene, ethanol, ethyl acetate, methyl acetate, propyl acetate, butyl acetate, ethers, ketones or mineral spirits; wherein the mass ratio of the pigment to the carrier resin to the solvent is (5-10): (30-90): (100-60).

The term "solvent bottle" as used herein refers to a glass bottle for holding a solid or liquid reagent having a mouth diameter less than or equal to the body diameter, such as, but not limited to, a wide or narrow mouth bottle, a ground, non-ground or screw-top bottle, a glass bottle with or without graduations.

The invention has the advantages that: 1. the system runs in a closed manner, vacuum drying is carried out, the operation environment is improved, small-batch treatment is carried out, and the efficiency is high; 2. the method is safe and environment-friendly, avoids material leakage, and reduces the flammable and explosive danger level of chemicals; 3. the solvent, the coloring resin and the like in the solvent bottle are recycled, and the regenerated pre-dispersible plastic color master batch is widely applied to the field of plastic cement, so that the additional value of a coloring resin product is greatly improved; 4. the grinding media such as glass bottles, glass beads and the like are thoroughly cleaned, so that the grinding media are prevented from being directly discharged or buried as hazardous wastes, the ecological environment is improved, and the sustainable utilization and development of resources are really realized.

Drawings

FIG. 1 is a schematic diagram of a solvent bottle recycling apparatus for a pigment according to example 1.1.

Fig. 2 is a block diagram of the vertical twin drum mixer of example 1.1.

Wherein, 1 is vertical twin-tub agitator, 11 is outer bucket, 12 is liftable interior bucket, 13 is the motor, 14 is the (mixing) shaft, 15 is the first pan feeding mouth of vertical twin-tub agitator, 16 is the first discharge gate of vertical twin-tub agitator, 17 is the first vacuum gas vent of vertical twin-tub agitator, 2 is the kneader, 3 is condensation equipment, 4 is first storage tank, 40 is the second pan feeding mouth of first storage tank, 41 is the second vacuum gas vent of first storage tank, 42 is the second discharge gate of first storage tank, 5 is the vacuum pump, 6 is the second storage tank.

Detailed Description

The invention provides a regeneration device and a regeneration method for a solvent bottle for pigment, which aim to solve the problems that the efficiency and the safety of the conventional solvent bottle cleaning device need to be improved, and no effective method is available for separation, recovery and regeneration treatment among pigment, solvent, resin, glass bottles and the like in the solvent bottle for pigment.

In a preferred embodiment, the present invention solves the above problems by:

(1) the explosion-proof variable frequency motor, the double-barrel vertical stirring and the stainless steel gauze isolation layer avoid the problems of mutual impact and solvent spin-drying during the batch processing of glass bottles;

(2) materials are sucked under negative pressure, and the materials are conveyed through a pipeline, so that the operating environment is improved;

(3) the medicament is used for dispersing, adsorbing and flocculating, so that leakage is avoided, and deflagration is prevented;

(4) the vacuum decompression closed operation avoids leakage, reduces the boiling point of the solvent and improves the operation safety;

(5) a kneading current relay is added to be linked with a temperature control system, so that the high temperature and the low temperature are automatically adjusted, and the danger level of a low-boiling-point solvent is reduced;

(6) a split oil bath circulating pump is adopted for heating, and the inflammable body and a heat source are electrically separated and distributed, so that the safety level is improved;

(7) the mixing, flocculation, kneading and distillation of a kneader are combined, so that the problems of solvent residue in low-temperature distillation resin and separation between the resin and a container are solved;

(8) blowing nitrogen is combined with holes on the surface of the inner barrel to form convection wind, so that residual solvent is blown off, and the physical and psychological health and safety of people are ensured;

(9) the color master batch is prepared by taking resin such as polyvinyl chloride and the like as a carrier, and is specially used in the field of plastics.

In another preferred embodiment, the process flow of the pigment recycling method of the present invention is as follows:

filling a solvent bottle into a barrel, adding a solvent → stirring and washing, pumping, spin-drying, blowing nitrogen → adding medicine, adsorbing, flocculating → kneading, distilling, discharging → separating and storing the solvent, recovering the solvent bottle and other media.

In another preferred embodiment, the pigment recycling method of the present invention comprises the steps of:

(1) a stirring and cleaning link: and (3) starting ventilation equipment, opening the cover of the solvent bottle in sequence, inversely filling the solvent bottle into an inner stirring barrel with the volume of 20-40 liters, and isolating each layer by using a stainless steel gauze, wherein the number of the gauzes is 5-30 meshes, so that the stable placement of the solvent bottle is ensured. The barrel body is made of stainless steel, 5-30 meshes of uniform holes are formed in the surface of the inner barrel, so that the convection of mobile phases such as a solvent in the barrel is guaranteed, the grinding medium is prevented from flowing into the outer barrel, the barrel cover with a silica gel pad is used for sealing and compacting, the lipid and the similar mixed solvent are added until the volume of two thirds of the barrel, the set rotating speed is 200-500rpm, and the stirring and washing are carried out for 1-5 minutes. And then, the solvent color paste generated by washing is pumped into a kneading machine or a second storage tank in vacuum until the solvent in the stirring barrel is emptied, and then the solvent is dried for 3-5 minutes in vacuum, and the process is circulated for three times to ensure that the solvent bottle is cleaned. And finally blowing nitrogen into the inner barrel to blow off the residual solvent, lifting the inner barrel, and taking out the clean glass bottle and the grinding medium to recycle.

(2) Adding medicine, kneading, dispersing and flocculating: and starting a vacuum pump and condensed water, and controlling the vacuum degree to be-0.02 to-0.045 MPa. Adding 100-150 g of medicament into a 5-10L kneader in advance, wherein the medicament comprises PVC paste resin, calcium carbonate, bentonite, magnesium stearate and the like, and the weight ratio is 100: 20-50: 10-30: adding the mixture into a kneader according to a ratio of 20-30 for kneading for 5 minutes, starting oil bath heating of the kneader, automatically setting the temperature to a low-temperature oil bath, carrying out low-temperature heating kneading distillation at 60-80 ℃, pumping the solvent color paste generated in the step 1 into the kneader for three times, controlling the ratio of the solvent color paste pumped for the first time to the medicament to be 25: (1-20) until the solvent color paste is completely dispersed, adsorbed and flocculated, so as to ensure that the material of the kneader is in a paste flocculation state during high-temperature distillation, and the material and the inner wall form a self-lubricating dispersion state, thereby avoiding material leakage, flammability and explosiveness in the mechanical sealing link.

(3) And (3) high-temperature kneading distillation: and (3) after the materials in the step (2) are dispersed and flocculated, distilling the low-boiling-point solvent, feeding the distillate into a first storage tank, starting to increase the stirring current, namely starting to work by a current relay after the stirring current of the kneader is increased to a set value, automatically adjusting a temperature control system to be a high-temperature oil bath, and performing high-temperature vacuum kneading at the temperature of 80-145 ℃ until all the solvent is removed by vacuum distillation and kneading. The distilled solvent can be recycled to the step 1 for reuse.

(4) And (3) color master recovery link: and (3) closing the kneader, heating, reducing the temperature of the kneader to 60-75 ℃ to enable the color master batch resin to be in a Microsoft state, taking out the solid coloring resin reclaimed material after the solvent is removed in the step (3), cooling, standing for 72-168 hours, and crushing into particles of 3mm by 5mm, namely selling the particles as pre-dispersed plastic color master batch.

In another preferred embodiment, the pigment recycling device and method of the present invention is achieved by the following key steps:

(1) the medicament is adopted for dispersing, adsorbing and flocculating, thereby avoiding leakage and preventing deflagration;

(2) an explosion-proof variable frequency motor is adopted, double cylinders are vertically stirred and dried, and a gauze isolation layer ensures cleanness, safety and stability;

(3) the inner cylinder surface with 5-30 meshes of micropores and a stainless steel gauze isolation layer are adopted, so that the cleaning efficiency is improved;

(4) negative pressure suction and pipeline conveying are adopted, so that the operating environment is improved;

(5) decompression kneading is adopted, the vacuum degree is controlled to be-0.02 to-0.045 MPa, leakage is avoided, and the boiling point of a solvent is reduced;

(6) the kneading current relay is added for control, and the high-low temperature oil bath distillation is adjusted;

(7) adopts a split oil bath circulating pump for heating, and the flammable body and the heat source are electrically separated and distributed, thereby improving the safety level

(8) The problems of resin viscosity and solvent residue are solved by combining the dispersion, flocculation and distillation of a kneading machine;

(9) blowing nitrogen is combined with holes on the surface of the inner barrel to blow off residual solvent, so that the physical and psychological health and safety of people are ensured;

(10) the plastic color master concentrate using resin as a carrier is prepared, and the problem of recycling of resin color paste is solved.

The apparatus and method for regenerating a solvent bottle for pigments according to the present invention will be further described with reference to the following specific examples.

In the following examples, the information on the instruments used is:

a kneader: the manufacturer: mechanical plant is mediated on Jiangsu Rugao well, model: NHZ-10.

Coating dispersion instrument: the manufacturer: hangzhou Xiaoshan shellfish, the type: GD-425

Computer colorimeter: united states HunterLab model ColorQuestXE

A plastic refining machine: tin-free double-image rubber-plastic machinery, SK-160

A vulcanizing machine: wuxi Sanyang machine, XLB-D350X 350

In the following examples, the information on the reagents used is shown in table 1 below:

EXAMPLE 1 regeneration apparatus for solvent bottle for pigment

Example 1.1

The structure of the solvent bottle recycling device for pigment in this example is shown in fig. 1, and includes the following parts:

(1) vertical double-barrel stirrer 1

The structure of the vertical double-barrel stirrer is shown in fig. 2, and comprises a base, a barrel body, a barrel cover and a motor 13 arranged outside the barrel body, wherein the barrel body comprises an outer barrel 11 and a liftable inner barrel 12, the motor 13 is connected with a stirring shaft 14, the stirring shaft 14 is arranged in the center of the barrel body, the end part of the stirring shaft is connected with the inner barrel 12, the inner barrel is driven to rotate through the rotation of the stirring shaft, more than one layer of gauze is horizontally arranged inside the inner barrel 11, small holes are uniformly formed in the barrel wall of the inner barrel 11, the outer barrel is provided with a first feeding hole 15 and a first discharging hole 16, and a first vacuum exhaust. Preferably, a sealing gasket is arranged at the joint of the barrel cover and the barrel body, and valves are arranged at the feeding port, the discharging port and the vacuum exhaust port.

Wherein, the volume of the outer barrel is 30-80L, the gauze is stainless steel gauze, the number of the gauze is 5-30 meshes, and the pores on the barrel wall of the inner barrel are 5-30 meshes. The volume of the inner barrel is 20-40L, and the ratio of the barrel diameter of the inner barrel to the barrel diameter of the outer barrel is 1: (1.2-1.4).

(2) Kneading machine 2

The kneader is provided with a kneading unit, a transmission unit, a heating unit, an electric control unit and a temperature control unit. The transmission unit comprises a motor and a paddle connected with the motor, the paddle comprises a main paddle and an auxiliary paddle, the heating unit comprises an oil bath circulating pump and is heated through oil bath, and the electric control unit comprises a current relay and can adjust the speed of the transmission unit; the temperature control unit comprises a temperature sensor arranged on the kneading unit and can monitor and regulate the temperature of the heating unit.

The material inlet of the kneading unit of the kneading machine 2 is connected with the first material outlet 16 of the vertical double-barrel stirrer, the material outlet of the kneading machine 2 is connected with the condensing equipment 3, and the material inlet and the material outlet of the kneading machine are both provided with valves. The volume of the kneading unit of the kneader 2 is 5-10L, and the temperature range of the heating unit is 60-145 ℃.

(3) Condensing plant 3

The feeding port of the condensing equipment 3 is connected with the discharge port of the kneading machine.

(4) First storage tank 4

The first storage tank 4 is provided with a second feeding port 40 at the top, a second vacuum exhaust port 41 at the top and a second discharge port 42 at the bottom. The second feeding port 40 is connected with the discharge port of the condensing device 3, the second vacuum exhaust port 41 is connected with the vacuum pump 5, and the second discharge port 42 is connected with the first feeding port 15 of the vertical double-barrel stirrer 1. And the feeding port, the discharging port and the vacuum exhaust port of the first storage tank are all provided with valves.

(5) Vacuum pump 5

The vacuum pump 5 is connected to the first vacuum exhaust port 17 of the vertical twin-tub agitator 1 and the second vacuum exhaust port 41 of the first storage tank 4. The inlet of the vacuum pump is provided with a valve.

Wherein the vacuum degree of the vacuum pump is-0.02 to-0.045 MPa.

(6) Second tank 6

A second storage tank 6 is arranged between the vertical double-barrel stirrer 1 and the first storage tank 4, the top and the bottom of the second storage tank are respectively provided with an upper discharge hole and a lower discharge hole, the lower discharge hole of the second storage tank 6 is connected with a first discharge hole 16 of the vertical double-barrel stirrer 1, and the upper discharge hole of the second storage tank 6 is connected with a second feed hole 40 of the first storage tank 4. And the upper exhaust port and the lower exhaust port of the second storage tank are provided with valves. Preferably, the upper vent valve of the second storage tank is an L-shaped three-way ball valve.

The use process of the device in the embodiment is as follows:

(1) placing the solvent bottle upside down on the gauze of the inner barrel of the vertical double-barrel stirrer 1, adding the mixed solvent from the first material inlet 15, starting the motor, rotating the stirring shaft to drive the inner barrel to rotate, and washing the solvent bottle;

(2) starting a vacuum pump, and pumping the obtained mixture containing the solvent and the color paste (the solvent color paste for short) into a kneader or a second storage tank 6 in vacuum until the solvent in the vertical double-barrel stirrer is emptied; the process can be repeated for a plurality of times properly to ensure that the solvent bottle is cleaned, nitrogen is blown into the vertical double-barrel stirrer to blow off the residual solvent, the inner barrel is lifted, and the clean solvent bottle is taken out;

(3) starting a kneading machine, adding a medicament, starting a vacuum pump and condensing equipment, uniformly mixing the medicament, setting the temperature of the kneading machine to be low-temperature oil bath, heating and kneading at low temperature (60-80 ℃), pumping the solvent color paste obtained by a vertical double-barrel stirrer into the kneading machine, heating and kneading at low temperature, distilling the solvent to obtain fraction, feeding the fraction into a first storage tank 4, adding the solvent color paste in batches, and controlling the mass ratio of the solvent color paste pumped for the first time to the medicament to be 25: (1-20), wherein the material level does not exceed 80% of the volume of the kneader at most until the solvent color paste is completely dispersed, adsorbed and flocculated;

the method for pumping the solvent color paste into the kneader can select any one of the following methods:

firstly, in the process of washing a solvent bottle by a vertical double-barrel stirrer, starting the kneader, adding a medicament, heating at low temperature for kneading, pumping the solvent color paste obtained in the vertical double-barrel stirrer into the kneader after the medicament is uniformly kneaded, closing a material inlet valve of the kneader when the addition of the solvent color paste in the kneader meets the requirement, opening a material outlet valve and an upper air outlet valve of a second storage tank 6, pumping the redundant solvent color paste into the second storage tank, and closing the material outlet valve of the second storage tank 6 and opening the material inlet valve of the kneader when the amount of the solvent color paste in the kneader is reduced, so that the solvent color paste in the second storage tank 6 is pumped into the kneader.

And secondly, in the process of washing the solvent bottle by the vertical double-barrel stirrer, starting a vacuum pump, closing a valve of a feeding port of the kneader 2, and opening a valve of a discharging port of the second storage tank 6, so that all the solvent color paste obtained in the vertical double-barrel stirrer is pumped into the second storage tank 6, after the medicine in the kneader is uniformly kneaded, closing a valve of an exhaust port on the second storage tank 6, and opening a valve of a feeding port of the kneader 2, so that the solvent color paste in the second storage tank 6 is pumped into the kneader.

(4) After the materials are completely dispersed and flocculated in the previous step, the solvent with low boiling point is distilled and enters a first storage tank 4; and (3) the stirring current begins to rise, namely after the stirring current of the kneader rises to a set value, the current relay starts to work, the temperature control system is adjusted to be a high-temperature oil bath, and high-temperature vacuum kneading is carried out at the temperature of 80-145 ℃ until all the solvent is distilled out.

(5) And (3) closing the heating function of the kneader to reduce the temperature to 60-75 ℃, taking out the reclaimed solid coloring resin after the solvent is removed in the previous step when the color master batch in the kneader is in a Microsoft state, cooling and standing for 72-168 hours (room temperature: 20-30 ℃), and crushing the reclaimed solid coloring resin to be sold as the disperse plastic color master batch.

Example 1.2

The structure of the regeneration device in this embodiment is similar to that in embodiment 1.1, wherein in the vertical twin-tub agitator, the volume of the outer tub is 52L, the volume of the inner tub is 30L, and the ratio of the inner tub to the outer tub is 1: 1.3, 4 layers of gauze are arranged in the inner barrel, the vertical distance between the gauzes is 100mm, the mesh number of the inner barrel is 30 meshes, and the pores on the barrel wall of the inner barrel are 30 meshes. The kneader manufacturer is a Jiangsu Rugao on-well kneading machinery factory with the model of NHZ-10; the size of the main paddle and the size of the auxiliary paddle in the kneader are both

The volume of the kneading unit in the kneader was 10L, and the stirring speed was 42 r/min.

Example 1.3

The structure of the regeneration device in this embodiment is similar to that in embodiment 1.1, wherein, in the vertical twin-tub agitator, the volume of the outer tub is 35L, the volume of the inner tub is 20L, and the ratio of the inner tub to the outer tub is 1: 1.3, 3 layers of gauze are arranged in the inner barrel, the vertical distance between the gauzes is 150mm, the mesh number of the gauze in the inner barrel is 20 meshes, and the pores on the wall of the inner barrel are 30 meshes.

EXAMPLE 2 regeneration of solvent bottle for pigment

Example 2.1

The solvent bottle regeneration apparatus for pigment described in example 1.2 was used, and the regeneration method was as follows:

(1) pretreatment link of solvent bottle

The dimensions of the solvent bottles used in this example were: the diameter of the bottle body is 6.5cm, the inner diameter of the bottle mouth is 5.2cm, the outer diameter of the bottle mouth is 5.8cm, and the height of the bottle is 8.3 cm. The solvent bottle is processed by the following steps:

adding 10g of phthalocyanine blue pigment (specification PB 15: 1), 90g of carrier resin 1 (solid content 35%), 10g of toluene and 100g of glass beads, covering a bottle cap, placing the bottle cap on a coating dispersion instrument, mixing and shaking for 3 hours to uniformly disperse the mixture, paving the mixture in the bottle, and simulating to prepare a solvent color paste system capable of detecting and evaluating the application performance of the ink or the paint.

(2) Stirring and cleaning link

And (3) starting ventilation equipment, sequentially opening the solvent bottles, reversely filling the solvent bottles into the inner barrel of the vertical double-barrel stirrer in the embodiment 1.2, isolating each layer by using a stainless steel gauze, wherein the gauze has 30 meshes, placing 3 layers, placing 12 solvent bottles in each layer, and ensuring the stable placement of the solvent bottles. Then, a barrel cover with a silica gel pad is used for sealing and compacting;

adding lipid and a mixed solvent of the same kind into a feeding port of a vertical double-barrel stirrer, wherein the components of the mixed solvent comprise propylene glycol methyl ether and ethyl acetate, the mass ratio is 1:20, the mixture is added into a barrel with the volume of two thirds, 12000g of the solvent is added, the set rotating speed is 200rpm, and the mixture is stirred and washed for 5 minutes. And then, pumping the solvent color paste generated by washing into a kneader in vacuum, temporarily pumping the redundant color paste into a second storage tank for storage until the solvent in the stirring barrel is emptied, and then performing vacuum spin-drying for 5 minutes, wherein the process is circulated for three times to ensure that the solvent bottle is cleaned. And finally blowing nitrogen into the inner barrel to blow off the residual solvent, lifting the inner barrel, and taking out the clean glass bottle and the grinding medium (glass beads) for recycling.

(3) Adding medicine, kneading, dispersing and flocculating link

And starting the vacuum pump and the condensed water to control the vacuum degree of the vacuum pump to be-0.02 MPa. 100g of the agent, consisting of PVC paste resin, calcium carbonate, bentonite and magnesium stearate, was added in advance to the kneader described in example 1.2, according to a 100: 20: 10: 20, starting oil bath heating of the kneader, setting the temperature to be a low-temperature oil bath, heating and kneading at the low temperature of 80 ℃, pumping the solvent color paste generated in the step (2) into the kneader, controlling the ratio of the solvent color paste pumped for the first time to the medicament to be 25:1, condensing the low fraction distilled out firstly, then feeding the low fraction into a first storage tank, pumping the solvent color paste stored in a second storage tank into a kneading machine for multiple times when the amount of the solvent color paste in the kneading machine is reduced, controlling the ratio of the solvent color paste to a medicament to be 25:1, controlling the material level to be not more than 80% of the solvent of the kneading machine at most, kneading for 15 minutes until the solvent color paste is completely dispersed, adsorbed and flocculated so as to ensure that the material of the kneading machine is in a paste flocculation state during high-temperature distillation, and the material and the inner wall form a self-lubricating dispersion state, thereby avoiding material leakage, flammability and explosiveness in a mechanical sealing link.

(4) High temperature kneading distillation link

And (3) after the materials in the step (2) are dispersed and flocculated, distilling the low-boiling-point solvent, starting to increase the stirring current, namely after the stirring current of the kneader is increased to a set value, starting to work by a current relay, adjusting a temperature control system to be a high-temperature oil bath, and performing high-temperature vacuum kneading at 135 ℃ until all the solvent is removed by vacuum distillation and kneading. The distilled solvent can be recycled to the step (2) and added into a vertical double-barrel stirrer for recycling.

(5) Color master recovery link

And (3) closing the kneader, heating, reducing the temperature of the kneader to 60 ℃ to enable the color master batch resin to be in a Microsoft state, taking out the color master batch resin reclaimed material after the solvent is removed in the step (4), cooling and standing for 72 hours, and crushing into particles of 3mm x 5mm, namely selling the particles as pre-dispersible plastic color master batch.

The obtained color master batch resin comprises phthalocyanine blue pigment, PVC paste resin, polyurethane resin, calcium carbonate, bentonite and magnesium stearate. The content of phthalocyanine blue in the color master batch resin is 22.6 percent.

Wherein, the formula for calculating the content of the phthalocyanine blue is as follows:

m1 is phthalocyanine blue pigment weight;

m2 is resin weight;

m3 is the weight of the medicament;

and C is the solid content of the resin.

The procedure was repeated three times and the average recovery of color concentrate was calculated to be 97.49% and the average tinctorial strength was calculated to be 99.97% (note: in the following examples, reference standards are compared using the color concentrate resin of group a of example 2.1 as a standard) as shown in table 2 below:

table 2 material testing data for example 2.1

The method for calculating the recovery rate comprises the following steps:

in the formula:

g-weight of solvent color paste, G

G1 weight of medicine, G

G2 color masterbatch resin weight, G

C-color paste concentration%

The method for detecting and calculating the tinting strength of the color master batch resin comprises the following steps: (refer to chemical industry standard HG/T4769.1-2014), the detection process is as follows:

weighing 1.0 g of color master batch resin, 65 g of PVC resin, 35 g of plasticizer DOP (dioctyl phthalate), 1 g of stearic acid, 2 g of barium stearate and 3 g of titanium dioxide, performing plastic refining molding on a two-roller machine at 155 ℃, performing plastic refining for 5 minutes, then vulcanizing on a vulcanizing machine at the temperature of 180 +/-2 ℃ for 30 seconds, preparing color card contrast, controlling the coloring power on a computer color measuring instrument after the color card is cooled, and expressing the contrast in percentage.

Example 2.2

(1) pretreatment link of solvent bottle

Similar to example 2.1, except that xylene was used as solvent and carrier resin 2 was used as carrier resin.

(2) Stirring and cleaning link

And (3) opening a ventilation device, opening the covers of the solvent bottles in sequence, and filling the solvent bottles in the inner barrel of the vertical double-barrel stirrer in the embodiment 1.2 in an inverted manner to ensure that the solvent bottles are stably placed. Then, a barrel cover with a silica gel pad is used for sealing and compacting;

adding lipid and a mixed solvent of the same kind from a feeding port of a vertical double-barrel stirrer, wherein the components of the mixed solvent comprise propylene glycol methyl ether and ethyl acetate in a mass ratio of 1:25 until the volume of the barrel is about 1/2, adding 10000g of the solvent in total, setting the rotating speed to be 500rpm, and stirring and washing for 1 minute. And then, the solvent color paste generated by washing is pumped into the second storage tank 6 in vacuum until the solvent in the stirring barrel is emptied, and then the solvent is dried for 5 minutes in vacuum, and the process is circulated for three times to ensure that the solvent bottle is cleaned. And finally blowing nitrogen into the inner barrel to blow off the residual solvent, lifting the inner barrel, and taking out the clean glass bottle and the grinding medium to recycle.

(3) Adding medicine, kneading, dispersing and flocculating link

And starting the vacuum pump and the condensed water to control the vacuum degree of the vacuum pump to be-0.035 MPa. 150g of a chemical consisting of polyvinyl chloride resin, calcium carbonate, bentonite and magnesium stearate was previously added to the kneader described in example 1.2, in a ratio of 100: 50: 30: 30 for 5 minutes, starting the oil bath heating of the kneader, automatically setting the temperature to a low-temperature oil bath, heating and kneading at 70 ℃, pumping the solvent color paste generated in the step (1) into the kneader for multiple times from a second storage tank, wherein the material level does not exceed 80 percent of the volume, and the ratio of the solvent color paste pumped for the first time to the medicament is controlled to be 25: 1.5, condensing the low fraction distilled firstly, and then putting the low fraction into a first storage tank, kneading for 20 minutes until the solvent color paste is completely dispersed, adsorbed and flocculated, so as to ensure that the material of the kneader is in a paste flocculation state during high-temperature distillation, and the material and the inner wall form a self-lubricating dispersion state, thereby avoiding material leakage, flammability and explosiveness in the mechanical sealing link.

(4) High temperature kneading distillation link

Analogously to example 2.1, the difference is that the high-temperature kneading temperature is 145 ℃.

(5) Color master recovery link

And (3) closing the kneader, heating, reducing the temperature of the kneader to 75 ℃ to enable the color master batch resin to be in a Microsoft state, taking out the solid coloring resin reclaimed material after the solvent is removed in the step (3), cooling, standing for 168 hours, and crushing into particles of 3mm by 5mm, thus being sold as pre-dispersible plastic color master batch.

The obtained color master batch resin comprises phthalocyanine blue pigment, PVC paste resin, chlorinated polypropylene resin, calcium carbonate, bentonite and magnesium stearate. The content of phthalocyanine blue in the color master batch resin is 21.89%.

The process is repeated for three times, and the average recovery rate of the recycled color master batch is 98.68 percent and the average tinting strength is 116.7 percent by calculation, which are shown in the following table 3:

table 3 material testing data for example 2.2

Example 2.3

(1) pretreatment link of solvent bottle

Same as example 2.1.

(2) Stirring and cleaning link

adding lipid and a mixed solvent of the same kind from a feeding port of a vertical double-barrel stirrer, wherein the components of the mixed solvent comprise ethylene glycol monomethyl ether and ethyl acetate, the mass ratio is 1:20, the mixture is added until the volume of about 1/2 of the barrel, 10000g of the solvent is added, the set rotating speed is 300rpm, and the mixture is stirred and washed for 1 minute. And then, vacuumizing the solvent color paste generated by washing into a second storage tank until the solvent in the stirring barrel is emptied, and performing vacuum drying for 5 minutes, wherein the process is circulated for three times to ensure that the solvent bottle is cleaned. And finally blowing nitrogen into the inner barrel to blow off the residual solvent, lifting the inner barrel, and taking out the clean glass bottle and the grinding medium to recycle.

(3) Adding medicine, kneading, dispersing and flocculating link

And starting the vacuum pump and the condensate water to control the vacuum degree of the vacuum pump to be-0.045 MPa. 150g of a pharmaceutical agent consisting of PVC paste resin, calcium carbonate, bentonite and magnesium stearate was added in advance to the kneader described in example 1.2, according to a 100: 35: 20: 25 for 5 minutes, starting oil bath heating of the kneader, setting the temperature to be a low-temperature oil bath, heating and kneading at 60 ℃, condensing the distilled fraction, then feeding the condensed fraction into a first storage tank, pumping the solvent color paste generated in the step 2 into the kneader for multiple times from a second storage tank, wherein the material level is not more than 80% of the volume, and the ratio of the solvent color paste pumped for the first time to the medicament is controlled to be 25: and 20, kneading for 20 minutes until the solvent color paste is completely dispersed, adsorbed and flocculated, so as to ensure that the material of the kneader is in a paste flocculation state during high-temperature distillation, and the material and the inner wall form a self-lubricating dispersion state, thereby avoiding material leakage, flammability and explosiveness in a mechanical sealing link.

(4) High temperature kneading distillation link

Analogously to example 2.1, the difference is that the high-temperature kneading temperature is 80 ℃.

(5) Color master recovery link

And (3) closing the kneader, heating, reducing the temperature of the kneader to 75 ℃ to enable the color master batch resin to be in a Microsoft state, taking out the solid coloring resin reclaimed material after the solvent is removed in the step (3), cooling and standing for 100 hours, and crushing into particles of 3mm by 5mm, thus being sold as pre-dispersible plastic color master batch.

The color master batch resin comprises phthalocyanine blue pigment, PVC paste resin, polyurethane resin, calcium carbonate, bentonite and magnesium stearate. The content of phthalocyanine blue in the color master batch resin is 21.89%.

The process is repeated for three times, and the average recovery rate of the recycled color master is 103.3 percent and the coloring power of the color master is 105.87 percent by calculation. See in particular table 4 below:

table 4 materials testing data for example 2.3

Example 2.4

(1) pretreatment link of solvent bottle

Same as example 2.2.

(2) Stirring and cleaning link

adding lipid and a mixed solvent of the same kind from a feeding port of a vertical double-barrel stirrer, wherein the components of the mixed solvent comprise propylene glycol methyl ether and ethyl acetate, the mass ratio is 1:15, the mixture is added until the volume of the mixture is about 1/2 of the barrel, 10000g of the solvent is added, the set rotating speed is 500rpm, and the mixture is stirred and washed for 1 minute. And then, the solvent color paste generated by washing is pumped into the second storage tank 6 in vacuum until the solvent in the stirring barrel is emptied, and then the solvent is dried for 5 minutes in vacuum, and the process is circulated for three times to ensure that the solvent bottle is cleaned. And finally blowing nitrogen into the inner barrel to blow off the residual solvent, lifting the inner barrel, and taking out the clean glass bottle and the grinding medium to recycle.

(3) Adding medicine, kneading, dispersing and flocculating link

And starting the vacuum pump and the condensed water to control the vacuum degree of the vacuum pump to be-0.035 MPa. 100g of a chemical agent consisting of polyvinyl chloride resin, calcium carbonate, bentonite and magnesium stearate was previously added to the kneader described in example 1.2, in a ratio of 100: 20: 10: 30 for 5 minutes, starting oil bath heating of the kneader, setting the temperature to be a low-temperature oil bath, heating and kneading at the low temperature of 80 ℃, condensing the distilled fraction, then feeding the condensed fraction into a first storage tank, pumping the solvent color paste generated in the step (1) into the kneader for multiple times from a second storage tank, wherein the material level is not more than 80 percent of the volume, and the ratio of the solvent color paste pumped for the first time to the medicament is controlled to be 25: and 5, kneading for 20 minutes until the solvent color paste is completely dispersed, adsorbed and flocculated, so as to ensure that the material of the kneader is in a paste flocculation state during high-temperature distillation, and the material and the inner wall form a self-lubricating dispersion state, thereby avoiding material leakage, flammability and explosiveness in a mechanical sealing link.

(4) High temperature kneading distillation link

Same as example 2.2.

(5) Color master recovery link

And (3) closing the kneader, heating, reducing the temperature of the kneader to 75 ℃ to enable the color master batch resin to be in a Microsoft state, taking out the solid coloring resin reclaimed material after the solvent is removed in the step (3), cooling and standing for 120 hours, and crushing into particles of 3mm by 5mm, thus being sold as pre-dispersible plastic color master batch. The color master batch resin comprises phthalocyanine blue pigment, chlorinated polypropylene resin, polyvinyl chloride resin, calcium carbonate, bentonite and magnesium stearate.

Wherein the content of phthalocyanine blue in the color master batch resin is 22.6 percent.

The process is repeated for three times, and the average recovery rate of the recycled color master batch is 98.8 percent and the average tinting strength of the color master batch resin is 123.3 percent by calculation. See in particular table 5 below:

table 5 materials testing data for example 2.4

Example 2.5

Example 2.5 is similar to example 2.1, except that:

the proportion of the mixed solvent in the step (2) is 1: 5; the Chinese medicinal preparation in the step (3) comprises PVC paste resin, calcium carbonate, bentonite and magnesium stearate, and the weight ratio of the PVC paste resin to the calcium carbonate to the bentonite to the magnesium stearate is 100: 40: 30: 40 mass ratio was added to the kneader to be kneaded.

The content of phthalocyanine blue in the color master batch resin is 22.6 percent, the average recovery rate of the recovered color master batch is 100.9 percent, and the average tinting strength of the color master batch is 86.4 percent. See in particular table 6 below:

table 6 materials testing data for example 2.5

Example 2.6

Example 2.6 is similar to example 2.1, except that:

the proportion of the mixed solvent in the step (2) is 1: 30, of a nitrogen-containing gas; the Chinese medicinal preparation in the step (3) comprises PVC paste resin, calcium carbonate, bentonite and magnesium stearate, and the weight ratio of the PVC paste resin to the calcium carbonate to the bentonite to the magnesium stearate is 100: 60: 40: 30 mass ratio was added to the kneader to knead.

The content of phthalocyanine blue in the color master batch resin is 22.6 percent, the average recovery rate of the recovered color master batch is 102.2 percent, and the average tinting strength of the color master batch resin is 84.4 percent. See in particular table 7 below:

table 7 materials testing data for example 2.6

Example 2.7

Example 2.7 is similar to example 2.1, except that: and (4) controlling the ratio of the solvent color paste pumped for the first time in the step (3) to the medicament to be 1: 1.

The content of phthalocyanine blue in the color master batch resin is 22.6 percent, the average recovery rate of the recovered color master batch is 98.2 percent, and the average tinting strength of the color master batch resin is 60.7 percent. See in particular table 8 below:

table 8 materials testing data for example 2.7

Example 2.8

Example 2.8 is similar to example 2.1, except that: the temperature of the low-temperature kneading was 80 ℃ and the temperature of the high-temperature kneading was 160 ℃.

The content of phthalocyanine blue in the color master batch resin is 22.6 percent, the average recovery rate of the recovered color master batch is 96.6 percent, and the average tinting strength of the color master batch resin is 90.8 percent. See in particular table 9 below:

table 9 materials testing data for example 2.8

In conclusion, the regeneration device is safe and environment-friendly, the solvent and the coloring resin in the solvent bottle can be recycled while the solvent bottle is cleaned, the additional value of the coloring resin product is greatly improved, and the sustainable utilization and development of resources are realized.

Claims

1. A solvent bottle regenerating device for pigments is characterized by comprising a vertical double-barrel stirrer (1), a kneading machine (2), a condensing device (3) and a first storage tank (4) which are communicated in sequence;

the vertical double-barrel stirrer comprises an outer barrel (11) and a liftable inner barrel (12), wherein more than one layer of gauze is horizontally arranged in the inner barrel (12), small holes are uniformly formed in the barrel wall of the inner barrel (12), the outer barrel (11) is provided with a first feeding hole (15) and a first discharging hole (16), and a first vacuum exhaust port (17) is formed in the top of the outer barrel (11);

the kneading machine (2) comprises a feeding port and a discharging port, the feeding port is connected with the discharging port of the vertical double-barrel stirrer, and the discharging port is connected with the condensing device;

a second feeding port (40) and a second vacuum exhaust port (41) are formed in the top of the first storage tank (4), a second discharging port (42) is formed in the bottom of the first storage tank (4), the second feeding port (40) of the first storage tank (4) is connected with the condensing equipment (3), and the second discharging port (42) of the first storage tank (4) is connected with the first feeding port (15) of the vertical double-barrel stirrer;

and a first vacuum exhaust port (17) of the vertical double-barrel stirrer and a second vacuum exhaust port (41) of the first storage tank are connected with a vacuum pump (5).

2. The regeneration device according to claim 1, wherein a second storage tank (6) is arranged between the vertical twin-tub agitator (1) and the first storage tank (4), the second storage tank (6) comprises a feed opening and an upper exhaust opening, the feed opening is connected with a first discharge opening (16) of the vertical twin-tub agitator, and the upper exhaust opening is connected with a second feed opening (40) of the first storage tank (4).

3. The recycling apparatus as claimed in claim 2, wherein the inlet of the kneader is provided with a valve, and the lower and upper outlets of the second tank are provided with valves.

4. The regeneration device of claim 3, wherein the upper vent valve of the second tank is a three-way ball valve.

5. The regeneration device according to claim 1 or 2, wherein the vertical twin-tub agitator (1) comprises a motor (13), the motor (13) is connected with an agitating shaft (14), the agitating shaft (14) is arranged in the center of the tub body, and the end of the agitating shaft (14) is connected with the inner tub (12).

6. The regeneration device of claim 3, wherein the vertical twin-tub agitator (1) comprises a motor (13), the motor (13) is connected with an agitating shaft (14), the agitating shaft (14) is arranged at the center of the tub, and the end of the agitating shaft (14) is connected with the inner tub (12).

7. The regeneration device of claim 4, wherein the vertical twin-tub agitator (1) comprises a motor (13), the motor (13) is connected with an agitating shaft (14), the agitating shaft (14) is arranged at the center of the tub, and the end of the agitating shaft (14) is connected with the inner tub (12).

8. The regeneration apparatus according to claim 1 or 2, wherein the ratio of the inner barrel diameter to the outer barrel diameter of the vertical twin-barrel agitator (1) is 1: (1.2-1.4).

9. The regeneration apparatus as claimed in claim 3, wherein the ratio of the inner drum diameter to the outer drum diameter of the vertical twin-drum agitator (1) is 1: (1.2-1.4).

10. The regeneration apparatus as claimed in claim 4, wherein the ratio of the inner drum diameter to the outer drum diameter of the vertical twin-drum agitator (1) is 1: (1.2-1.4).

11. The regeneration apparatus as claimed in claim 5, wherein the ratio of the inner drum diameter to the outer drum diameter of the vertical twin-drum agitator (1) is 1: (1.2-1.4).

12. The regeneration apparatus as claimed in claim 6, wherein the ratio of the inner drum diameter to the outer drum diameter of the vertical twin-drum agitator (1) is 1: (1.2-1.4).

13. The regeneration apparatus as claimed in claim 7, wherein the ratio of the inner drum diameter to the outer drum diameter of the vertical twin-drum agitator (1) is 1: (1.2-1.4).

14. The recycling apparatus according to claim 1 or 2, wherein the kneader is provided with a kneading unit, a transmission unit, a heating unit, an electric control unit, and a temperature control unit.

15. The recycling apparatus according to claim 3, wherein the kneader is provided with a kneading unit, a transmission unit, a heating unit, an electric control unit, and a temperature control unit.

16. The recycling apparatus according to claim 4, wherein the kneader is provided with a kneading unit, a transmission unit, a heating unit, an electric control unit, and a temperature control unit.

17. The recycling apparatus according to claim 5, wherein the kneader is provided with a kneading unit, a transmission unit, a heating unit, an electric control unit, and a temperature control unit.

18. The recycling apparatus according to claim 6, wherein the kneader is provided with a kneading unit, a transmission unit, a heating unit, an electric control unit, and a temperature control unit.

19. The recycling apparatus according to claim 7, wherein the kneader is provided with a kneading unit, a transmission unit, a heating unit, an electric control unit, and a temperature control unit.

20. The recycling apparatus according to claim 8, wherein the kneader is provided with a kneading unit, a transmission unit, a heating unit, an electric control unit, and a temperature control unit.

21. The recycling apparatus according to claim 9, wherein the kneader is provided with a kneading unit, a transmission unit, a heating unit, an electric control unit, and a temperature control unit.

22. The recycling apparatus according to claim 10, wherein the kneader is provided with a kneading unit, a transmission unit, a heating unit, an electric control unit, and a temperature control unit.

23. The recycling apparatus according to claim 11, wherein the kneader is provided with a kneading unit, a transmission unit, a heating unit, an electric control unit, and a temperature control unit.

24. The recycling apparatus according to claim 12, wherein the kneader is provided with a kneading unit, a transmission unit, a heating unit, an electric control unit, and a temperature control unit.

25. The recycling apparatus according to claim 13, wherein the kneader is provided with a kneading unit, a transmission unit, a heating unit, an electric control unit, and a temperature control unit.

26. A method for regenerating a solvent bottle for pigments, comprising the steps of:

(1) solvent bottle washing process: opening the regeneration device of claim 1, uniformly placing the solvent bottle upside down on the gauze in the inner barrel of the vertical double-barrel stirrer (1), adding the mixed solvent, and washing the solvent bottle to obtain a mixture of the solvent and the color paste; starting a vacuum pump, pumping the obtained solvent and color paste mixture into a kneader, lifting an inner barrel, and taking out a clean solvent bottle;

27. The recycling method according to claim 26, wherein in the step (2), the mass ratio of the solvent and color paste mixture and the medicament which are firstly added into the kneader is 25: (1-20).

28. The recycling method according to claim 26 or 27, wherein in the step (1), the solvent and color paste mixture obtained by the vertical twin-tub agitator is pumped into a kneader or a second storage tank.

29. The regeneration method of claim 26 or 27, wherein the mixed solvent in the step (1) comprises alcohol ether and ester, and the mass ratio of the alcohol ether to the ester is 1 (10-25).

30. The regeneration method of claim 28, wherein the mixed solvent in the step (1) comprises alcohol ether and ester, and the mass ratio of the alcohol ether to the ester is 1 (10-25).

31. The regeneration method according to claim 26 or 27, wherein the mixed solvent in step (1) comprises an alcohol ether and an ester, wherein the alcohol ether is selected from one or more of propylene glycol methyl ether, ethylene glycol methyl ether, diethylene glycol methyl ether, triethylene glycol methyl ether, ethylene glycol monopropyl ether and diethylene glycol monopropyl ether, and the ester is selected from one or more of ethyl acetate, methyl acetate, propyl acetate, butyl acetate, diethylene glycol propyl ether acetate and propylene glycol ethyl ether acetate.

32. The regeneration method according to claim 28, wherein the mixed solvent in step (1) comprises an alcohol ether and an ester, wherein the alcohol ether is one or more selected from propylene glycol methyl ether, ethylene glycol methyl ether, diethylene glycol methyl ether, triethylene glycol methyl ether, ethylene glycol monopropyl ether and diethylene glycol monopropyl ether, and the ester is one or more selected from ethyl acetate, methyl acetate, propyl acetate, butyl acetate, diethylene glycol propyl ether acetate and propylene glycol ethyl ether acetate.

33. The recycling method according to claim 26 or 27, wherein the degree of vacuum of the kneader in step (2) and step (3) is set to-0.02 to-0.045 MPa.

34. The recycling method according to claim 28, wherein the degree of vacuum of the kneader in the step (2) and the step (3) is set to-0.02 to-0.045 MPa.

35. The recycling method according to claim 29, wherein the degree of vacuum of the kneader in the step (2) and the step (3) is set to-0.02 to-0.045 MPa.

36. The recycling method according to claim 30, wherein the degree of vacuum of the kneader in the step (2) and the step (3) is set to-0.02 to-0.045 MPa.

37. The recycling method according to claim 31, wherein the degree of vacuum of the kneader in the step (2) and the step (3) is set to-0.02 to-0.045 MPa.

38. The recycling method according to claim 32, wherein the degree of vacuum of the kneader in the step (2) and the step (3) is set to-0.02 to-0.045 MPa.

39. The recycling method according to claim 26 or 27, wherein the pharmaceutical agent in step (2) comprises resin, calcium carbonate, bentonite and magnesium stearate in a mass ratio of 100: (20-50): (10-30): (20-30); the resin is selected from one or more of PVC paste resin, polyvinyl chloride resin, polyurethane resin and chlorinated polypropylene resin.

40. The recycling method according to claim 28, wherein the pharmaceutical agent in step (2) comprises resin, calcium carbonate, bentonite and magnesium stearate in a mass ratio of 100: (20-50): (10-30): (20-30); the resin is selected from one or more of PVC paste resin, polyvinyl chloride resin, polyurethane resin and chlorinated polypropylene resin.

41. The recycling method according to claim 29, wherein the pharmaceutical agent in step (2) comprises resin, calcium carbonate, bentonite and magnesium stearate in a mass ratio of 100: (20-50): (10-30): (20-30); the resin is selected from one or more of PVC paste resin, polyvinyl chloride resin, polyurethane resin and chlorinated polypropylene resin.

42. The recycling method according to claim 30, wherein the pharmaceutical agent in step (2) comprises resin, calcium carbonate, bentonite and magnesium stearate in a mass ratio of 100: (20-50): (10-30): (20-30); the resin is selected from one or more of PVC paste resin, polyvinyl chloride resin, polyurethane resin and chlorinated polypropylene resin.

43. The recycling method according to claim 31, wherein the pharmaceutical agent in step (2) comprises resin, calcium carbonate, bentonite and magnesium stearate in a mass ratio of 100: (20-50): (10-30): (20-30); the resin is selected from one or more of PVC paste resin, polyvinyl chloride resin, polyurethane resin and chlorinated polypropylene resin.

44. The recycling method according to claim 32, wherein the pharmaceutical agent in step (2) comprises resin, calcium carbonate, bentonite and magnesium stearate in a mass ratio of 100: (20-50): (10-30): (20-30); the resin is selected from one or more of PVC paste resin, polyvinyl chloride resin, polyurethane resin and chlorinated polypropylene resin.

45. The recycling method according to claim 33, wherein the pharmaceutical agent in step (2) comprises resin, calcium carbonate, bentonite and magnesium stearate in a mass ratio of 100: (20-50): (10-30): (20-30); the resin is selected from one or more of PVC paste resin, polyvinyl chloride resin, polyurethane resin and chlorinated polypropylene resin.

46. The recycling method according to claim 34, wherein the pharmaceutical agent in step (2) comprises resin, calcium carbonate, bentonite and magnesium stearate in a mass ratio of 100: (20-50): (10-30): (20-30); the resin is selected from one or more of PVC paste resin, polyvinyl chloride resin, polyurethane resin and chlorinated polypropylene resin.

47. The recycling method according to claim 35, wherein the pharmaceutical agent in step (2) comprises resin, calcium carbonate, bentonite and magnesium stearate in a mass ratio of 100: (20-50): (10-30): (20-30); the resin is selected from one or more of PVC paste resin, polyvinyl chloride resin, polyurethane resin and chlorinated polypropylene resin.

48. The recycling method according to claim 36, wherein the pharmaceutical agent in step (2) comprises resin, calcium carbonate, bentonite and magnesium stearate in a mass ratio of 100: (20-50): (10-30): (20-30); the resin is selected from one or more of PVC paste resin, polyvinyl chloride resin, polyurethane resin and chlorinated polypropylene resin.

49. The recycling method according to claim 37, wherein the pharmaceutical agent in step (2) comprises resin, calcium carbonate, bentonite and magnesium stearate in a mass ratio of 100: (20-50): (10-30): (20-30); the resin is selected from one or more of PVC paste resin, polyvinyl chloride resin, polyurethane resin and chlorinated polypropylene resin.

50. The recycling method according to claim 38, wherein the pharmaceutical agent in step (2) comprises resin, calcium carbonate, bentonite and magnesium stearate in a mass ratio of 100: (20-50): (10-30): (20-30); the resin is selected from one or more of PVC paste resin, polyvinyl chloride resin, polyurethane resin and chlorinated polypropylene resin.

51. The recycling method according to claim 26 or 27, wherein the color concentrate recycling process of step (4) comprises the steps of: and (4) closing the kneader, taking out the materials in the kneader when the temperature is reduced to 60-75 ℃, cooling and standing for 72-168 hours to obtain the color master.

52. The recycling method of claim 28, wherein the color concentrate recycling process of step (4) comprises the steps of: and (4) closing the kneader, taking out the materials in the kneader when the temperature is reduced to 60-75 ℃, cooling and standing for 72-168 hours to obtain the color master.

53. The recycling method of claim 29, wherein the color concentrate recycling process of step (4) comprises the steps of: and (4) closing the kneader, taking out the materials in the kneader when the temperature is reduced to 60-75 ℃, cooling and standing for 72-168 hours to obtain the color master.

54. The recycling method of claim 30, wherein the color concentrate recycling process of step (4) comprises the steps of: and (4) closing the kneader, taking out the materials in the kneader when the temperature is reduced to 60-75 ℃, cooling and standing for 72-168 hours to obtain the color master.

55. The recycling method of claim 31, wherein the color concentrate recycling process of step (4) comprises the steps of: and (4) closing the kneader, taking out the materials in the kneader when the temperature is reduced to 60-75 ℃, cooling and standing for 72-168 hours to obtain the color master.

56. The recycling method of claim 32, wherein the color concentrate recycling process of step (4) comprises the steps of: and (4) closing the kneader, taking out the materials in the kneader when the temperature is reduced to 60-75 ℃, cooling and standing for 72-168 hours to obtain the color master.

57. The recycling method of claim 33, wherein the color concentrate recycling process of step (4) comprises the steps of: and (4) closing the kneader, taking out the materials in the kneader when the temperature is reduced to 60-75 ℃, cooling and standing for 72-168 hours to obtain the color master.

58. The recycling method of claim 34, wherein the color concentrate recycling process of step (4) comprises the steps of: and (4) closing the kneader, taking out the materials in the kneader when the temperature is reduced to 60-75 ℃, cooling and standing for 72-168 hours to obtain the color master.

59. The recycling method of claim 35, wherein the color concentrate recycling process of step (4) comprises the steps of: and (4) closing the kneader, taking out the materials in the kneader when the temperature is reduced to 60-75 ℃, cooling and standing for 72-168 hours to obtain the color master.

60. The recycling method of claim 36, wherein the color concentrate recycling process of step (4) comprises the steps of: and (4) closing the kneader, taking out the materials in the kneader when the temperature is reduced to 60-75 ℃, cooling and standing for 72-168 hours to obtain the color master.

61. The recycling method of claim 37, wherein the color concentrate recycling process of step (4) comprises the steps of: and (4) closing the kneader, taking out the materials in the kneader when the temperature is reduced to 60-75 ℃, cooling and standing for 72-168 hours to obtain the color master.

62. The recycling method of claim 38, wherein the color concentrate recycling process of step (4) comprises the steps of: and (4) closing the kneader, taking out the materials in the kneader when the temperature is reduced to 60-75 ℃, cooling and standing for 72-168 hours to obtain the color master.

63. The recycling method of claim 39, wherein the color concentrate recycling process of step (4) comprises the steps of: and (4) closing the kneader, taking out the materials in the kneader when the temperature is reduced to 60-75 ℃, cooling and standing for 72-168 hours to obtain the color master.

64. The recycling method of claim 40, wherein the color concentrate recycling process of step (4) comprises the steps of: and (4) closing the kneader, taking out the materials in the kneader when the temperature is reduced to 60-75 ℃, cooling and standing for 72-168 hours to obtain the color master.

65. The recycling method of claim 41, wherein the color concentrate recycling process of step (4) comprises the steps of: and (4) closing the kneader, taking out the materials in the kneader when the temperature is reduced to 60-75 ℃, cooling and standing for 72-168 hours to obtain the color master.

66. The recycling method of claim 42, wherein the color concentrate recycling process of step (4) comprises the steps of: and (4) closing the kneader, taking out the materials in the kneader when the temperature is reduced to 60-75 ℃, cooling and standing for 72-168 hours to obtain the color master.

67. The recycling method of claim 43, wherein the color concentrate recycling process of step (4) comprises the steps of: and (4) closing the kneader, taking out the materials in the kneader when the temperature is reduced to 60-75 ℃, cooling and standing for 72-168 hours to obtain the color master.

68. The recycling method of claim 44, wherein the color concentrate recycling process of step (4) comprises the steps of: and (4) closing the kneader, taking out the materials in the kneader when the temperature is reduced to 60-75 ℃, cooling and standing for 72-168 hours to obtain the color master.

69. The recycling method of claim 45, wherein the color concentrate recycling process of step (4) comprises the steps of: and (4) closing the kneader, taking out the materials in the kneader when the temperature is reduced to 60-75 ℃, cooling and standing for 72-168 hours to obtain the color master.

70. The recycling method of claim 46, wherein the color concentrate recycling process of step (4) comprises the steps of: and (4) closing the kneader, taking out the materials in the kneader when the temperature is reduced to 60-75 ℃, cooling and standing for 72-168 hours to obtain the color master.

71. The recycling method of claim 47, wherein the color concentrate recycling process of step (4) comprises the steps of: and (4) closing the kneader, taking out the materials in the kneader when the temperature is reduced to 60-75 ℃, cooling and standing for 72-168 hours to obtain the color master.

72. The recycling method of claim 48, wherein the color concentrate recycling process of step (4) comprises the steps of: and (4) closing the kneader, taking out the materials in the kneader when the temperature is reduced to 60-75 ℃, cooling and standing for 72-168 hours to obtain the color master.

73. The recycling method of claim 49, wherein the color concentrate recycling process of step (4) comprises the steps of: and (4) closing the kneader, taking out the materials in the kneader when the temperature is reduced to 60-75 ℃, cooling and standing for 72-168 hours to obtain the color master.

74. The recycling method of claim 50, wherein the color concentrate recycling process of step (4) comprises the steps of: and (4) closing the kneader, taking out the materials in the kneader when the temperature is reduced to 60-75 ℃, cooling and standing for 72-168 hours to obtain the color master.