CN112076696A - Preparation system and preparation method of polycarboxylate superplasticizer macromonomer raw material initiator - Google Patents
Preparation system and preparation method of polycarboxylate superplasticizer macromonomer raw material initiator Download PDFInfo
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- CN112076696A CN112076696A CN202010954554.0A CN202010954554A CN112076696A CN 112076696 A CN112076696 A CN 112076696A CN 202010954554 A CN202010954554 A CN 202010954554A CN 112076696 A CN112076696 A CN 112076696A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/02—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/68—Preparation of metal alcoholates
- C07C29/70—Preparation of metal alcoholates by converting hydroxy groups to O-metal groups
Abstract
A preparation system and a preparation method of a polycarboxylate superplasticizer macromonomer raw material initiator are disclosed, wherein the preparation system comprises a chain initiator preparation kettle, a circulating pump, a circulating heat exchanger, a catalyst feeding tank and a solid-liquid mixing reactor; wherein, the top end of the chain initiator preparation kettle is provided with a first nitrogen purge valve and a first vent valve; the bottom is provided with a kettle bottom valve; the chain initiator preparation kettle is communicated with the top end of the solid-liquid mixing reactor through a gas phase pipeline and is communicated with the bottom of the solid-liquid mixing reactor through a liquid phase pipeline, a discharge port of the chain initiator preparation kettle is communicated with a circulating pump through a circulating inlet pipeline, a discharge end of the circulating pump is communicated with a circulating heat exchanger through a first circulating outlet pipeline, and the top end of the circulating heat exchanger is communicated with the solid-liquid mixing reactor through a second circulating outlet pipeline; two rubber gloves are arranged on the side wall of the catalyst feeding tank, and a feeding port at the bottom is communicated with the solid-liquid mixing reactor through a catalyst feeding pipeline. The system does not need a stirring device, is simple to operate and has high safety factor.
Description
Technical Field
The invention relates to the technical field of polycarboxylic acid water reducing agents, in particular to a system and a method for preparing a macromonomer raw material initiator of a polycarboxylic acid water reducing agent.
Background
At present, the preparation of the raw material initiator of the macromonomer of the polycarboxylic acid water reducing agent mainly adopts the following three methods, (1) sodium methoxide reacts with raw material alcohol to prepare the chain initiator, the reaction is mild, but methanol is generated, which is very unfavorable for the quality of the macromonomer of the water reducing agent, so that the by-product methanol is required to be completely removed from the system through a rectifying tower, and the by-product can be stably and efficiently removed by accurately controlling the pressure and the temperature in the tower, so that the purity of the chain initiator is greatly improved, the preparation time is prolonged, and the production cost is increased. (2) The chain-forming initiator is prepared by reacting the powdery alkali metal compound with the raw material alcohol, and although the chain-forming initiator prepared by reacting the powdery alkali metal compound with the raw material alcohol does not generate moisture and does not need vacuum dehydration, the reaction is violent in the preparation process of the initiator, hydrogen is generated, the risk is high, the initiator is easy to catch fire and cause explosion, and many accidents have occurred in domestic production enterprises. (3) Solid alkali metal reacts with raw material alcohol to prepare a chain-forming initiator for alkoxylation reaction; the method is to react solid alkali metal with raw material alcohol in a stirring kettle, and although the reaction is mild, a mechanical transmission stirring device in the equipment is still a great unsafe factor due to the existence of hydrogen.
Disclosure of Invention
In view of the above technical problems and disadvantages, a first object of the present invention is to provide a system for preparing a raw material starter of a macromonomer of a polycarboxylate superplasticizer, which completes the preparation of the raw material starter of the macromonomer of the polycarboxylate superplasticizer through a cyclic reaction, and has the advantages of no need of a stirring device in the whole process, simple operation and high safety factor.
In order to realize the purpose, the invention is realized by adopting the following technical scheme;
a system for preparing a polycarboxylate superplasticizer macromonomer raw material initiator comprises a chain initiator preparation kettle, a circulating pump, a circulating heat exchanger, a catalyst feeding tank and a solid-liquid mixing reactor; a raw material alcohol feeding valve is mounted on a feeding port of the chain initiator preparation kettle, the feeding port is communicated with raw material alcohol through a feeding pipeline, and a mass flow meter is arranged on the feeding pipeline and used for monitoring the quality of the fed alcohol; the top end of the chain initiator configuration kettle is provided with a nitrogen gas inlet and a gas outlet, the nitrogen gas inlet is provided with a first nitrogen purging valve, and the gas outlet is provided with a first emptying valve; a discharge hole is formed in the bottom of the chain initiator preparation kettle, and a kettle bottom valve is mounted on the discharge hole; the chain initiator preparation kettle is communicated with the top end of the solid-liquid mixing reactor through a gas phase pipeline, and a gas phase communicating valve is arranged on the gas phase pipeline; the chain initiator preparation kettle is communicated with the bottom of the solid-liquid mixing reactor through a liquid phase pipeline, and a liquid phase outlet valve is arranged on the liquid phase pipeline; the discharge hole of the chain initiator preparation kettle is communicated with a circulating pump through a circulating inlet pipeline, and a circulating pump inlet valve is arranged on the circulating inlet pipeline;
the discharge end of the circulating pump is communicated with the circulating heat exchanger through a first discharge and circulation pipeline, a circulating pump outlet regulating valve is arranged on the first discharge and circulation pipeline, the first discharge and circulation pipeline is communicated with an initiator discharge pipe, and an initiator discharge valve is arranged on the initiator discharge pipe;
the circulating heat exchanger is used for cooling liquid in the heat exchanger according to a heat exchange principle, and the top end of the circulating heat exchanger is communicated with the solid-liquid mixing reactor through a second outlet circulating pipeline;
a feeding port is formed in one side of the catalyst feeding tank, a nitrogen inlet and an exhaust port are formed in the top end of the catalyst feeding tank, a second nitrogen purge valve is mounted on the nitrogen inlet, a second vent valve is mounted on the exhaust port, two rubber glove ports and a sight glass are arranged on the side wall of the catalyst feeding tank, rubber gloves are mounted on the rubber glove ports, and sleeve ports of the rubber gloves are sleeved on the rubber glove ports to be in closed connection; the bottom of the catalyst feeding tank is provided with a feeding port, the feeding port is provided with a catalyst feeding valve, and the feeding port is communicated with the solid-liquid mixing reactor through a catalyst feeding pipeline.
Preferably, the chain initiator configuration kettle is further provided with a temperature transmitter, a liquid level transmitter and a pressure transmitter, wherein the temperature transmitter is used for monitoring the temperature in the chain initiator configuration kettle, the liquid level transmitter is used for monitoring the height of liquid in the chain initiator configuration kettle, and the pressure transmitter is used for monitoring the pressure in the chain initiator configuration kettle.
Preferably, a water inlet is formed in the side wall of the bottom of the circulating heat exchanger, a circulating water regulating valve is mounted on the water inlet, the water inlet is communicated with the cooling liquid through a water inlet pipe, a water outlet is formed in the side wall of the top end of the circulating heat exchanger, a circulating water outlet valve is mounted on the water outlet, and the water outlet is connected with a water outlet pipe; and a circulating temperature transmitter is arranged on the second circulating outlet pipeline and controls the temperature through the circulating temperature transmitter.
Preferably, the bottom of the catalyst throwing tank is provided with a first clean discharge port, and a clean discharge valve is mounted on the first clean discharge port; and a second drain port is formed in the circulating pump, and a circulating pump drain valve is installed on the second drain port.
The second purpose of the invention is to provide a preparation method of the polycarboxylate superplasticizer macromonomer raw material initiator, which is simple and safe, low in reaction temperature, short in reaction time and low in production cost.
A preparation method of a polycarboxylate superplasticizer macromonomer raw material initiator comprises the following steps:
step 1, putting prepared solid catalyst metal sodium into a catalyst putting tank through a putting port, then closing the putting port, opening a nitrogen purge valve for purging, and performing nitrogen replacement on the catalyst putting tank;
and 4, after the reaction is finished, opening a liquid outlet valve, returning the materials to the chain initiator preparation kettle through a liquid phase pipeline, then opening the circulating pump again for reaction, repeatedly performing the circulating reaction until the reaction is finished, and opening an initiator discharge valve.
As a preferred mode of the invention, the open of the vent valve on the chain initiator preparation kettle is kept between 5 and 20Kpa, and the circulating temperature is controlled between 40 and 45 ℃ during the whole circulating reaction process.
The invention has the advantages and beneficial effects that:
(1) the preparation system provided by the invention is simple to operate and high in safety coefficient, after the raw material alcohol and the metal sodium are put in, the cyclic reaction can be realized by controlling the circulating pump subsequently, the preparation of the polycarboxylate superplasticizer macromonomer raw material initiator can be completed through the cyclic reaction, a stirring device is not needed in the whole process, and hydrogen generated in the reaction process can be discharged in time, so that the safety is greatly improved.
(2) The preparation method provided by the invention is simple and safe, and has the advantages of low reaction temperature, short reaction time and low production cost.
Drawings
FIG. 1 is a schematic view of the overall configuration of a production system of the present invention;
FIG. 2 is a schematic view of the installation of rubber gloves on a catalyst delivery canister according to the present invention.
Reference numerals: a chain initiator preparation kettle 1, a circulating pump 2, a circulating heat exchanger 3, a catalyst feeding tank 4, a solid-liquid mixing reactor 5, a feeding pipeline 11, a gas phase pipeline 12, a liquid phase pipeline 13, a feeding and circulating pipeline 14, a first discharging and circulating pipeline 15, an initiator discharging pipe 16, a second discharging and circulating pipeline 17, a catalyst feeding pipeline 18, a raw material alcohol feeding valve 101, a first nitrogen purge valve 102, a first emptying valve 103, a kettle bottom valve 104, a temperature transmitter 105, a liquid level transmitter 106, a pressure transmitter 107, a mass flowmeter 111, a gas phase communication valve 121, a liquid outlet valve 131, a circulating pump inlet valve 141, a circulating pump outlet regulating valve 151, an initiator discharging valve 161, a circulating temperature transmitter 171, a circulating pump drain valve 201, a circulating water regulating valve 301, a circulating water outlet valve 302, a second nitrogen purge valve 401, a second emptying valve 402, a rubber glove port 403, a sight glass 404, a rubber glove 405, A catalyst dosing valve 406, a purge valve 407.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Referring to fig. 1 and fig. 2, the system for preparing the polycarboxylate superplasticizer macromonomer raw material initiator provided by the invention comprises a chain initiator preparation kettle 1, a circulating pump 2, a circulating heat exchanger 3, a catalyst feeding tank 4 and a solid-liquid mixing reactor 5; a raw material alcohol feeding valve 101 is installed on a feeding port of the chain initiator preparation kettle 1, the feeding port is communicated with raw material alcohol through a feeding pipeline 11, a mass flow meter 111 is arranged on the feeding pipeline 11, and the mass flow meter 111 is used for monitoring the mass of the fed alcohol; the top end of the chain initiator configuration kettle is provided with a nitrogen gas inlet and a gas outlet, the nitrogen gas inlet is provided with a first nitrogen purging valve 102, and the gas outlet is provided with a first gas release valve 103; a discharge hole is formed in the bottom of the chain initiator preparation kettle, and a kettle bottom valve 104 is mounted on the discharge hole; the chain initiator configuration kettle is also provided with a temperature transmitter 105, a liquid level transmitter 106 and a pressure transmitter 107, wherein the temperature transmitter 105 is used for monitoring the temperature in the chain initiator configuration kettle, the liquid level transmitter 106 is used for monitoring the height of liquid in the chain initiator configuration kettle, and the pressure transmitter 107 is used for monitoring the pressure in the chain initiator configuration kettle; the chain initiator preparation kettle 1 is communicated with the top end of the solid-liquid mixing reactor 5 through a gas phase pipeline 12, and a gas phase communicating valve 121 is arranged on the gas phase pipeline 12; the chain initiator preparation kettle 1 is communicated with the bottom of the solid-liquid mixing reactor 5 through a liquid phase pipeline 13, and a liquid outlet valve 131 is arranged on the liquid phase pipeline 13; the discharge hole of the chain initiator preparation kettle 1 is communicated with a circulating pump 2 through a circulating inlet pipeline 14, and a circulating pump inlet valve 141 is arranged on the circulating inlet pipeline 14;
the discharge end of the circulating pump 2 is communicated with the circulating heat exchanger 3 through a first discharge circulating pipeline 15, a circulating pump outlet regulating valve 151 is installed on the first discharge circulating pipeline 15, the first discharge circulating pipeline 15 is communicated with an initiator discharge pipe 16, and an initiator discharge valve 161 is installed on the initiator discharge pipe 16; a second drain port is further formed in the circulating pump 2, and a circulating pump drain valve 201 is mounted on the second drain port;
a water inlet is formed in the side wall of the bottom of the circulating heat exchanger 3, a circulating water regulating valve 301 is installed on the water inlet, the water inlet is communicated with cooling liquid through a water inlet pipe, a water outlet is formed in the side wall of the top end of the circulating heat exchanger, a circulating water outlet valve 302 is installed on the water outlet, the water outlet is connected with a water outlet pipe, the circulating heat exchanger 3 is used for cooling liquid in the circulating heat exchanger 3 through the heat exchange principle, and the top end of the circulating heat exchanger 3 is communicated with the solid-liquid mixing reactor 5 through a second circulating; a circulating temperature transmitter 171 is installed on the second outlet circulation pipeline 17, and the temperature is controlled by the circulating temperature transmitter 171;
a feeding port is formed in one side of the catalyst feeding tank 4, a nitrogen gas inlet and an exhaust port are formed in the top end of the catalyst feeding tank, a second nitrogen purge valve 401 is installed on the nitrogen gas inlet, a second vent valve 402 is installed on the exhaust port, two rubber glove ports 403 and a viewing mirror 404 are formed in the side wall of the catalyst feeding tank, rubber gloves 405 are installed on the rubber glove ports, and sleeve ports of the rubber gloves are sleeved on the rubber glove ports to be hermetically connected (the sleeve ports can be tightly pressed through flanges and sealing rings and then fixed through bolts); a feeding port is arranged at the bottom of the catalyst feeding tank, a catalyst feeding valve 406 is arranged on the feeding port, and the feeding port is communicated with the solid-liquid mixing reactor 5 through a catalyst feeding pipeline 18; the bottom of jar is put in to catalyst still is provided with first clean mouth, install the blow-off valve 407 on the first clean mouth.
Example 2
The method for preparing the polycarboxylate superplasticizer macromonomer raw material initiator by using the preparation system comprises the following steps:
step 1, putting prepared solid catalyst metal sodium (17.5kg) into a catalyst putting tank 4 through a putting port, then closing the putting port, opening a second nitrogen purge valve 401 for purging, performing nitrogen replacement on the catalyst putting tank, and completely discharging air in the catalyst putting tank;
and 4, after the surface reaction of the raw material alcohol and the metal sodium is finished (about 4 hours), opening the liquid outlet valve 131, returning the materials to the chain initiator preparation kettle 1 through the liquid phase pipeline 13, then opening the circulating pump 2 again for reaction, repeatedly performing the circulating reaction until the reaction is finished (whether the reaction of the catalyst is finished or not can be judged according to the temperature change of the materials in the chain initiator preparation kettle), and opening the initiator discharge valve.
Claims (6)
1. A preparation system of a polycarboxylate superplasticizer macromonomer raw material initiator is characterized by comprising a chain initiator preparation kettle, a circulating pump, a circulating heat exchanger, a catalyst feeding tank and a solid-liquid mixing reactor; a raw material alcohol feeding valve is mounted on a feeding port of the chain initiator preparation kettle, the feeding port is communicated with raw material alcohol through a feeding pipeline, and a mass flow meter is arranged on the feeding pipeline and used for monitoring the quality of the fed alcohol; the top end of the chain initiator configuration kettle is provided with a nitrogen gas inlet and a gas outlet, the nitrogen gas inlet is provided with a first nitrogen purging valve, and the gas outlet is provided with a first emptying valve; a discharge hole is formed in the bottom of the chain initiator preparation kettle, and a kettle bottom valve is mounted on the discharge hole; the chain initiator preparation kettle is communicated with the top end of the solid-liquid mixing reactor through a gas phase pipeline, and a gas phase communicating valve is arranged on the gas phase pipeline; the chain initiator preparation kettle is communicated with the bottom of the solid-liquid mixing reactor through a liquid phase pipeline, and a liquid phase outlet valve is arranged on the liquid phase pipeline; the discharge hole of the chain initiator preparation kettle is communicated with a circulating pump through a circulating inlet pipeline, and a circulating pump inlet valve is arranged on the circulating inlet pipeline;
the discharge end of the circulating pump is communicated with the circulating heat exchanger through a first discharge and circulation pipeline, a circulating pump outlet regulating valve is arranged on the first discharge and circulation pipeline, the first discharge and circulation pipeline is communicated with an initiator discharge pipe, and an initiator discharge valve is arranged on the initiator discharge pipe;
the circulating heat exchanger is used for cooling liquid in the heat exchanger according to a heat exchange principle, and the top end of the circulating heat exchanger is communicated with the solid-liquid mixing reactor through a second outlet circulating pipeline;
a feeding port is formed in one side of the catalyst feeding tank, a nitrogen inlet and an exhaust port are formed in the top end of the catalyst feeding tank, a second nitrogen purge valve is mounted on the nitrogen inlet, a second vent valve is mounted on the exhaust port, two rubber glove ports and a sight glass are arranged on the side wall of the catalyst feeding tank, rubber gloves are mounted on the rubber glove ports, and sleeve ports of the rubber gloves are sleeved on the rubber glove ports to be in closed connection; the bottom of the catalyst feeding tank is provided with a feeding port, the feeding port is provided with a catalyst feeding valve, and the feeding port is communicated with the solid-liquid mixing reactor through a catalyst feeding pipeline.
2. The system for preparing the polycarboxylate water reducer macromonomer raw material initiator as claimed in claim 1, wherein a temperature transmitter, a liquid level transmitter and a pressure transmitter are further arranged on the chain initiator configuration kettle, the temperature transmitter is used for monitoring the temperature in the chain initiator configuration kettle, the liquid level transmitter is used for monitoring the height of liquid in the chain initiator configuration kettle, and the pressure transmitter is used for monitoring the pressure in the chain initiator configuration kettle.
3. The system for preparing the raw material starter of the macromonomer of the water reducing agent for polycarboxylic acid according to claim 1, wherein a water inlet is provided on a side wall of the bottom of the circulation heat exchanger, a circulating water regulating valve is installed on the water inlet, the water inlet is communicated with a coolant through a water inlet pipe, a water outlet is provided on a side wall of the top end of the circulation heat exchanger, a circulating water outlet valve is installed on the water outlet, and the water outlet is connected with a water outlet pipe; and a circulating temperature transmitter is arranged on the second circulating outlet pipeline and controls the temperature through the circulating temperature transmitter.
4. The system for preparing the polycarboxylate superplasticizer macromonomer raw material starter according to claim 1, wherein a first purge port is provided at the bottom of the catalyst feeding tank, and a purge valve is installed on the first purge port; and a second drain port is formed in the circulating pump, and a circulating pump drain valve is installed on the second drain port.
5. A preparation method of a polycarboxylate superplasticizer macromonomer raw material initiator is characterized by comprising the following steps:
step 1, putting prepared solid catalyst metal sodium into a catalyst putting tank through a putting port, then closing the putting port, opening a nitrogen purge valve for purging, and performing nitrogen replacement on the catalyst putting tank;
step 2, opening a catalyst feeding valve, wearing rubber gloves on both hands, then stretching into a catalyst feeding tank, and feeding the solid catalyst metal sodium in the catalyst feeding tank into the solid-liquid mixing reactor through a sight glass;
step 3, feeding raw material alcohol into a chain initiator preparation kettle through a feeding pipeline, closing a raw material alcohol feeding valve when a mass flow meter shows that the raw material alcohol entering the chain initiator preparation kettle reaches a feeding amount, opening a kettle bottom valve, starting a circulating pump, feeding the raw material alcohol into the circulating heat exchanger through the circulating pump, cooling through the circulating heat exchanger, reacting with solid-liquid mixed reactor and solid catalyst metal sodium, opening a gas phase communication valve on a gas phase pipeline all the time in the reaction process, discharging hydrogen generated in the reaction process into the chain initiator preparation kettle through the gas phase pipeline, and discharging through an emptying valve on the chain initiator preparation kettle;
and 4, after the reaction is finished, opening a liquid outlet valve, returning the materials to the chain initiator preparation kettle through a liquid phase pipeline, then opening the circulating pump again for reaction, repeatedly performing the circulating reaction until the reaction is finished, and opening an initiator discharge valve.
6. The method for preparing the polycarboxylate water reducer macromonomer raw material starter as claimed in claim 5, wherein an emptying valve on the chain starter preparation kettle is opened and maintained at 5-20Kpa, and the circulating temperature is controlled at 40-45 ℃ in the whole circulating reaction process.
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Effective date of registration: 20210408 Address after: 132000 41 Yumen street, Longtan District, Jilin City, Jilin Province Applicant after: Yu Guangchen Address before: No.77, Xinsheng street, Chuanying District, Jilin City, Jilin Province 132000 Applicant before: JILIN CHEMICAL GROUP OIL GREASE CHEMICAL Co.,Ltd. |
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Application publication date: 20201215 |