CN111530435B - Polyurethane soft foam adsorption material internally wrapped with chrysotile nanotubes and preparation method thereof - Google Patents
Polyurethane soft foam adsorption material internally wrapped with chrysotile nanotubes and preparation method thereof Download PDFInfo
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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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
- B01J20/265—Synthetic macromolecular compounds modified or post-treated polymers
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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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
- C08G18/76—Polyisocyanates or polyisothiocyanates cyclic aromatic
- C08G18/7614—Polyisocyanates or polyisothiocyanates cyclic aromatic containing only one aromatic ring
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
- C08K7/26—Silicon- containing compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
Abstract
The invention discloses a polyurethane soft foam adsorption material internally wrapped with chrysotile nanotubes and a preparation method thereof, relating to the technical field of industrial wastewater treatment, and the polyurethane soft foam adsorption material comprises the following components in parts by mass: 43-45 parts of polyether polyol, 14-19 parts of toluene diisocyanate (TDI80/20), 1-1.5 parts of water, 330.11-0.13 part of triethylene diamine A, 0.07-0.12 part of stannous octoate (T-9), 0.35-0.44 part of an organic silicon foam stabilizer and 35-40 parts of chrysotile nanotubes; the polyurethane foam is internally coated with the chrysotile nanotube by utilizing the characteristics of more pores and large surface area, so that pollutants such as heavy metal ions, anions (clusters) and the like can be effectively removed, and the application investment cost is reduced. The adsorption material prepared by the invention can be repeatedly used after desorption treatment when adsorption is saturated.
Description
Technical Field
The invention relates to the technical field of sewage treatment, in particular to a preparation method of an adsorption material, and particularly relates to a polyurethane flexible foam adsorption material internally wrapped with chrysotile nanotubes and a preparation method thereof.
Background
The polyurethane soft foam plastic has excellent physical and mechanical properties, acoustic properties, electrical properties and chemical resistance, and can be used for preparing terminal products with various properties and purposes by changing the chemical structure, specification, variety and other adjustment formula combinations of raw materials during the synthesis of polyurethane. The chrysotile nanotube is a novel nano material, overcomes the defects that natural chrysotile has uneven pipe diameter, more accompanying minerals and difficult purification, and part of the pipes are internally provided with fillers, has special chemical activity and surface properties, can be used for adsorbing and removing environmental pollutants such as heavy metal ions and anions (clusters), and has low treatment cost, better compatibility with the environment and high efficiency. While the single polyurethane soft foam plastic can not adsorb heavy metal ions, the chrysotile nanotube is a good adsorbing material, but has good dispersibility in aqueous solution, which brings great difficulty to the solid-liquid separation process in the adsorption treatment, and the application of the chrysotile nanotube in the field of wastewater treatment is limited.
Chinese patent application No. CN201310409695.4 discloses a method for preparing a magnetic chrysotile nanotube, which adopts the technical scheme that a magnetic material is loaded on the surface of the chrysotile nanotube, and then the magnetic material is recovered by a magnetic separation technology. However, the following defects still exist in the practical use process of the patent: the magnetic substance loaded on the surface of the serpentine nanotube partially reduces the adsorption performance of the serpentine nanotube, and in addition, the magnetic separation cannot achieve one hundred percent recovery, and meanwhile, the magnetic separation process needs to be additionally provided with corresponding magnetic separation equipment.
The magnetic substance loaded on the surface of the serpentine nanotube partially reduces the adsorption performance of the serpentine nanotube, so that no study on the combination of two adsorption materials, namely the chrysotile nanotube and the polyurethane soft foam is made, and how to combine the two adsorption materials, namely the chrysotile nanotube and the polyurethane soft foam, is the direction of efforts of technicians in the field.
Disclosure of Invention
The invention aims to: the invention provides a polyurethane flexible foam adsorption material internally wrapped with chrysotile nanotubes and a preparation method thereof, aiming at solving the technical problem of combining two adsorption materials, namely chrysotile nanotubes and polyurethane flexible foam.
The invention specifically adopts the following technical scheme for realizing the purpose:
the polyurethane soft foam adsorption material internally wrapped with the chrysotile nanotubes comprises the following components in parts by mass: 43-45 parts of polyether polyol, 14-19 parts of toluene diisocyanate (TDI80/20), 1-1.5 parts of water and triethylene diamine A330.11-0.13 part of stannous octoate (T-9), 0.07-0.12 part of organic silicon foam stabilizer, 0.35-0.44 part of organic silicon foam stabilizer and 35-40 parts of chrysotile nanotube.
Preferably, 43.5 parts of polyether polyol, 19 parts of toluene diisocyanate (TDI80/20), 1.5 parts of water and triethylene diamine A330.13 part, 0.09 part of stannous octoate (T-9), 0.44 part of organosilicon foam stabilizer and 35 parts of chrysotile nanotubes.
Preferably, the polyether polyol is 44 parts, the toluene diisocyanate (TDI80/20) is 17 parts, the water is 1.2 parts, and the triethylene diamine A330.12 part, 0.07 part of stannous octoate (T-9), 0.40 part of organosilicon foam stabilizer and 38 parts of chrysotile nanotube.
Preferably, the polyether polyol is 44.5 parts, the toluene diisocyanate (TDI80/20) is 14 parts, the water is 1.0 part, and the triethylene diamine A330.11 part of stannous octoate (T-9), 0.35 part of organic silicon foam stabilizer and 40 parts of chrysotile nanotube.
The preparation method of the polyurethane flexible foam adsorption material internally wrapped with the chrysotile nanotube comprises the following steps:
step 1, material preparation: weighing 43-45 parts of polyether polyol, 14-19 parts of toluene diisocyanate (TDI80/20), 1-1.5 parts of water, 330.11-0.13 part of triethylene diamine A, 0.07-0.12 part of stannous octoate (T-9), 0.35-0.44 part of organic silicon foam stabilizer and 35-40 parts of chrysotile nanotube for later use.
Step 2, at room temperature, uniformly mixing polyether polyol with the chrysotile nanotubes, and standing for 24 hours for later use;
step 3, mixing water, triethylene diamine and an organic silicon foam stabilizer in a first mixing cylinder, and stirring for 30min at the rotating speed of 1000r/min by using an electric control mechanical stirrer to fully and uniformly mix:
step 4, mixing the mixture of the polyether polyol and the chrysotile nanotube with stannous octoate in a second mixing barrel, and stirring for 15min at a high speed by using an electric control mechanical stirrer;
and 5, mixing the prepared small samples in the first mixing cylinder and the second mixing cylinder with toluene diisocyanate (TDI80/20), stirring at a high speed for 3-5 s, pouring into a mold, freely foaming at the temperature of 25 ℃, curing the materials for 10min, and preparing the polyurethane soft foam adsorption material internally wrapped with the chrysotile nanotubes.
Preferably, the polyether polyol is polyether 330.
The preparation method of the chrysotile nanotube comprises the following steps:
step a, mixing 40 parts of active MgO and nano SiO2Sequentially adding 23 parts of the mixture into a hydrothermal reaction kettle, and then adding distilled water accounting for 70% of the total volume of the reaction kettle;
step b, adjusting the pH value of the reaction system to 13 by using NaOH solution;
step c, heating the hydrothermal reaction kettle to 220 ℃ and reacting for 72 hours at constant temperature;
and d, naturally cooling to room temperature after the reaction is finished, filtering the reaction solution, washing a filter cake to be neutral by using distilled water, and drying at a constant temperature of 105 ℃ to obtain the chrysotile nanotube.
The invention has the following beneficial effects:
1. the polyurethane foam is internally coated with the chrysotile nanotube due to the characteristics of more pores and large surface area, so that pollutants such as heavy metal ions, anions (clusters) and the like can be effectively removed, the problem of difficult solid-liquid separation in the treatment of the powder adsorbing material is not needed to be considered, separation equipment such as magnetic separation and the like is not needed to be added, and the investment cost of application is reduced. The adsorption material prepared by the invention can be repeatedly used after desorption treatment when the adsorption is saturated, has excellent market value and environmental protection value, and can be widely popularized and applied in the water treatment industry.
Detailed Description
The following examples further describe the invention in detail in order that those skilled in the art may better understand the invention.
Example 1
The preparation method of the polyurethane flexible foam adsorption material internally wrapped with the chrysotile nanotube comprises the following steps:
step 1, material preparation: 33043.5 parts of polyether, 19 parts of toluene diisocyanate (TDI80/20), 1.5 parts of water and triethylene diamine A330.13 part, 0.09 part of stannous octoate (T-9), 0.44 part of organosilicon foam stabilizer and 35 parts of chrysotile nanotube for standby.
Step 2, at room temperature, uniformly mixing polyether 330 and chrysotile nanotubes, and standing for 24 hours for later use;
step 3, mixing water, triethylene diamine and an organic silicon foam stabilizer in a first mixing cylinder, and stirring for 30min at the rotating speed of 1000r/min by using an electric control mechanical stirrer to fully and uniformly mix:
step 4, mixing the mixture of the polyether 330 and the chrysotile nanotube with stannous octoate in a second mixing barrel, and stirring for 15min at a high speed by using an electric control mechanical stirrer;
and 5, mixing the prepared small samples in the first mixing cylinder and the second mixing cylinder with toluene diisocyanate (TDI80/20), stirring at a high speed for 3-5 s, pouring into a mold, freely foaming at the temperature of 25 ℃, curing the materials for 10min, and preparing the polyurethane soft foam adsorption material internally wrapped with the chrysotile nanotubes.
The preparation method of the chrysotile nanotube comprises the following steps:
step a, mixing 40 parts of active MgO and nano SiO2Sequentially adding 23 parts of the mixture into a hydrothermal reaction kettle, and then adding distilled water accounting for 70% of the total volume of the reaction kettle;
step b, adjusting the pH value of the reaction system to 13 by using NaOH solution;
step c, heating the hydrothermal reaction kettle to 220 ℃ and reacting for 72 hours at constant temperature;
and d, naturally cooling to room temperature after the reaction is finished, filtering the reaction solution, washing a filter cake to be neutral by using distilled water, and drying at a constant temperature of 105 ℃ to obtain the chrysotile nanotube.
Example 2
The preparation method of the polyurethane flexible foam adsorption material internally wrapped with the chrysotile nanotube comprises the following steps:
step 1, material preparation: weighing 33044 parts of polyether, 17 parts of toluene diisocyanate (TDI80/20), 1.2 parts of water and triethylene diamine A330.12 part, 0.07 part of stannous octoate (T-9), 0.40 part of organosilicon foam stabilizer and 38 parts of chrysotile nanotube for later use.
Step 2, at room temperature, uniformly mixing polyether 330 and chrysotile nanotubes, and standing for 24 hours for later use;
step 3, mixing water, triethylene diamine and an organic silicon foam stabilizer in a first mixing cylinder, and stirring for 30min at the rotating speed of 1000r/min by using an electric control mechanical stirrer to fully and uniformly mix:
step 4, mixing the mixture of the polyether 330 and the chrysotile nanotube with stannous octoate in a second mixing barrel, and stirring for 15min at a high speed by using an electric control mechanical stirrer;
and 5, mixing the prepared small samples in the first mixing cylinder and the second mixing cylinder with toluene diisocyanate (TDI80/20), stirring at a high speed for 3-5 s, pouring into a mold, freely foaming at the temperature of 25 ℃, curing the materials for 10min, and preparing the polyurethane soft foam adsorption material internally wrapped with the chrysotile nanotubes.
The preparation method of the chrysotile nanotube comprises the following steps:
step a, mixing 40 parts of active MgO and nano SiO2Sequentially adding 23 parts of the mixture into a hydrothermal reaction kettle, and then adding distilled water accounting for 70% of the total volume of the reaction kettle;
step b, adjusting the pH value of the reaction system to 13 by using NaOH solution;
step c, heating the hydrothermal reaction kettle to 220 ℃ and reacting for 72 hours at constant temperature;
and d, naturally cooling to room temperature after the reaction is finished, filtering the reaction solution, washing a filter cake to be neutral by using distilled water, and drying at a constant temperature of 105 ℃ to obtain the chrysotile nanotube.
Example 3
The preparation method of the polyurethane flexible foam adsorption material internally wrapped with the chrysotile nanotube comprises the following steps:
step 1, material preparation: 33044.5 parts of polyether, 14 parts of toluene diisocyanate (TDI80/20), 1.0 part of water and triethylene diamine A330.11 part of stannous octoate (T-9), 0.35 part of organic silicon foam stabilizer and 40 parts of chrysotile nanotube for standby.
Step 2, at room temperature, uniformly mixing polyether 330 and chrysotile nanotubes, and standing for 24 hours for later use;
step 3, mixing water, triethylene diamine and an organic silicon foam stabilizer in a first mixing cylinder, and stirring for 30min at the rotating speed of 1000r/min by using an electric control mechanical stirrer to fully and uniformly mix:
step 4, mixing the mixture of the polyether 330 and the chrysotile nanotube with stannous octoate in a second mixing barrel, and stirring for 15min at a high speed by using an electric control mechanical stirrer;
and 5, mixing the prepared small samples in the first mixing cylinder and the second mixing cylinder with toluene diisocyanate (TDI80/20), stirring at a high speed for 3-5 s, pouring into a mold, freely foaming at the temperature of 25 ℃, curing the materials for 10min, and preparing the polyurethane soft foam adsorption material internally wrapped with the chrysotile nanotubes.
The preparation method of the chrysotile nanotube comprises the following steps:
step a, mixing 40 parts of active MgO and nano SiO2Sequentially adding 23 parts of the mixture into a hydrothermal reaction kettle, and then adding distilled water accounting for 70% of the total volume of the reaction kettle;
step b, adjusting the pH value of the reaction system to 13 by using NaOH solution;
step c, heating the hydrothermal reaction kettle to 220 ℃ and reacting for 72 hours at constant temperature;
and d, naturally cooling to room temperature after the reaction is finished, filtering the reaction solution, washing a filter cake to be neutral by using distilled water, and drying at a constant temperature of 105 ℃ to obtain the chrysotile nanotube.
The above description is only a preferred embodiment of the present invention, and not intended to limit the present invention, the scope of the present invention is defined by the appended claims, and all equivalent changes made by applying the contents of the description of the present invention should be embraced in the scope of the present invention.
Claims (6)
1. The polyurethane soft foam adsorption material internally wrapped with the chrysotile nanotube is characterized in that: the adhesive comprises the following components in parts by mass: 43-45 parts of polyether polyol, 14-19 parts of toluene diisocyanate, 1-1.5 parts of water and triethylene diamine A330.11-0.13 part of stannous octoate, 0.07-0.12 part of organic silicon foam stabilizer, 0.35-0.44 part of organic silicon foam stabilizer and 35-40 parts of chrysotile nanotube;
the preparation method of the material comprises the following steps:
step 1, material preparation: weighing 43-45 parts of polyether polyol, 14-19 parts of toluene diisocyanate, 1-1.5 parts of water and triethylene diamine A330.11-0.13 part of stannous octoate, 0.07-0.12 part of organic silicon foam stabilizer, 0.35-0.44 part of organic silicon foam stabilizer and 35-40 parts of chrysotile nanotube for later use;
step 2, at room temperature, uniformly mixing polyether polyol with the chrysotile nanotubes, and standing for 24 hours for later use;
step 3, mixing water, triethylene diamine and an organic silicon foam stabilizer in a first mixing cylinder, and stirring for 30min at the rotating speed of 1000r/min by using an electric control mechanical stirrer to fully and uniformly mix:
step 4, mixing the mixture of the polyether polyol and the chrysotile nanotube with stannous octoate in a second mixing barrel, and stirring for 15min at a high speed by using an electric control mechanical stirrer;
and 5, mixing the prepared small samples in the first mixing cylinder and the second mixing cylinder with toluene diisocyanate, stirring at a high speed for 3-5 s, pouring into a mold, freely foaming at the temperature of 25 ℃, curing the materials for 10min, and preparing the polyurethane soft foam adsorbing material internally wrapped with the chrysotile nanotubes.
2. The polyurethane flexible foam adsorbent material containing chrysotile nanotubes as claimed in claim 1, wherein: 43.5 parts of polyether polyol, 19 parts of toluene diisocyanate, 1.5 parts of water and triethylene diamine A330.13 part, 0.09 part of stannous octoate, 0.44 part of organic silicon foam stabilizer and 35 parts of chrysotile nanotube.
3. The polyurethane flexible foam adsorbent material containing chrysotile nanotubes as claimed in claim 1, wherein: 44 parts of polyether polyol, 17 parts of toluene diisocyanate, 1.2 parts of water and triethylene diamine A330.12 part, 0.07 part of stannous octoate, 0.40 part of organic silicon foam stabilizer and 38 parts of chrysotile nanotube.
4. The polyurethane flexible foam adsorbent material containing chrysotile nanotubes as claimed in claim 1, wherein: 44.5 parts of polyether polyol, 14 parts of toluene diisocyanate, 1.0 part of water and triethylene diamine A330.11 part, 0.11 part of stannous octoate, 0.35 part of organic silicon foam stabilizer and 40 parts of chrysotile nanotube.
5. The polyurethane flexible foam adsorbent material containing chrysotile nanotubes as claimed in claim 1, wherein: the polyether polyol is polyether 330.
6. The polyurethane flexible foam adsorbent material containing chrysotile nanotubes as claimed in claim 1, wherein: in step 1, the preparation method of the chrysotile nanotube comprises the following steps:
step a, mixing 40 parts of active MgO and nano SiO2Sequentially adding 23 parts of the mixture into a hydrothermal reaction kettle, and then adding distilled water accounting for 70% of the total volume of the reaction kettle;
step b, adjusting the pH value of the reaction system to 13 by using NaOH solution;
step c, heating the hydrothermal reaction kettle to 220 ℃ and reacting for 72 hours at constant temperature;
and d, naturally cooling to room temperature after the reaction is finished, filtering the reaction solution, washing a filter cake to be neutral by using distilled water, and drying at a constant temperature of 105 ℃ to obtain the chrysotile nanotube.
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