CN112280287A - Preparation method of polyurethane thermal insulation material - Google Patents
Preparation method of polyurethane thermal insulation material Download PDFInfo
- Publication number
- CN112280287A CN112280287A CN202011187844.3A CN202011187844A CN112280287A CN 112280287 A CN112280287 A CN 112280287A CN 202011187844 A CN202011187844 A CN 202011187844A CN 112280287 A CN112280287 A CN 112280287A
- Authority
- CN
- China
- Prior art keywords
- parts
- thermal insulation
- insulation material
- reaction kettle
- polyurethane thermal
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
- C08J9/12—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent
- C08J9/14—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent organic
- C08J9/141—Hydrocarbons
-
- 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
- C08G18/4804—Two or more polyethers of different physical or chemical nature
-
- 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
- C08G18/7657—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings
- C08G18/7664—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings containing alkylene polyphenyl groups
- C08G18/7671—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings containing alkylene polyphenyl groups containing only one alkylene bisphenyl group
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0061—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof characterized by the use of several polymeric components
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0066—Use of inorganic compounding ingredients
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/009—Use of pretreated compounding ingredients
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2203/00—Foams characterized by the expanding agent
- C08J2203/14—Saturated hydrocarbons, e.g. butane; Unspecified hydrocarbons
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2375/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
- C08J2375/04—Polyurethanes
- C08J2375/08—Polyurethanes from polyethers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2405/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2401/00 or C08J2403/00
- C08J2405/04—Alginic acid; Derivatives thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2405/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2401/00 or C08J2403/00
- C08J2405/08—Chitin; Chondroitin sulfate; Hyaluronic acid; Derivatives thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2483/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2483/04—Polysiloxanes
Abstract
The invention discloses a preparation method of a polyurethane thermal insulation material, belonging to the technical field of thermal insulation materials and comprising the following steps: (1) preparing a heat preservation reinforcing agent, (2) weighing raw materials, and (3) mixing. The method has simple integral steps and is easy to popularize and apply, and the prepared polyurethane thermal insulation material has the characteristics of good thermal insulation, stable use quality, safety, environmental protection and the like.
Description
Technical Field
The invention belongs to the technical field of heat insulation materials, and particularly relates to a preparation method of a polyurethane heat insulation material.
Background
As one of the heat insulating materials with the best performance at present, foam pores of polyurethane foam plastic are mainly closed, have lower heat conductivity coefficient, lower density, certain strength and hardness, have excellent electrical properties and sound insulation and shock resistance effects, can improve flame retardance, water resistance and corrosion resistance after being treated by an additive, and are widely applied to industries such as automobiles, buildings, refrigerators, furniture, packaging, shipbuilding, petrochemical engineering and the like. Due to the characteristics of extremely low thermal conductivity, low water resistance, small density, high specific strength, easy cutting and the like, the composite material has the advantages of being applied to heat preservation of refrigerators and refrigerated cabinets, heat preservation of pipelines on roof, walls, windows, floors and the like in the building industry, heat preservation and cold insulation of pipelines and pipes for water, steam and the like in the industry and being incomparable with other traditional materials.
With the continuous expansion of application scenes and the continuous improvement of material performance requirements of people, the existing polyurethane heat-insulating material needs to be continuously improved and enhanced in heat-insulating property and other characteristics.
Disclosure of Invention
The invention aims to provide a preparation method of a polyurethane thermal insulation material, which aims to overcome the defects in the prior art.
The technical scheme adopted by the invention is as follows:
a preparation method of a polyurethane thermal insulation material comprises the following steps:
(1) preparing a heat preservation reinforcing agent:
1) carrying out irradiation treatment on the attapulgite in an ultraviolet irradiation box, and taking out for later use after 22-26 min;
2) mixing sodium alginate, chitosan and acetic acid-sodium acetate solution, putting into a reaction kettle, continuously stirring for 4-6 h, adding excessive calcium chloride solution into the reaction kettle, continuously stirring for 3-5 h, filtering, washing the filtrate with deionized water to neutrality, and finally putting into a drying oven for drying for 50-60 min to obtain a composite material A for later use;
3) mixing polycaprolactone, anhydrous dimethyl sulfoxide and nano carbon powder, putting into a stirring tank, and stirring and dissolving uniformly to obtain a composite material B for later use;
4) mixing attapulgite treated in the operation 1), the composite material A obtained in the operation 2) and the composite material B obtained in the operation 3) together, putting the mixture into a reaction kettle, filling nitrogen into the reaction kettle, heating to keep the temperature in the reaction kettle at 78-83 ℃, continuously stirring for 2.5-3.5 hours, rapidly cooling the reaction kettle to 20-23 ℃, adding an excessive ethanol solution into the reaction kettle, filtering, putting the filtrate into a vacuum drying oven for drying for 2-3 hours, and taking out the filtrate to obtain a heat preservation reinforcing agent for later use;
(2) weighing raw materials:
weighing the following raw materials in parts by weight for later use:
70-75 parts of diphenylmethane diisocyanate, 35-45 parts of plant fiber-based polyether polyol, 20-35 parts of plant oil-based polyether polyol, 2-4 parts of a catalyst, 1-3 parts of an organic flame retardant, 0.5-1.5 parts of a foaming agent, 1-4 parts of silicone oil, 5-8 parts of a heat preservation reinforcing agent prepared in the step (1) and 7-10 parts of deionized water;
(3) mixing treatment:
mixing diphenylmethane diisocyanate, plant fiber-based polyether polyol and plant oil-based polyether polyol together, then adding a catalyst, an organic flame retardant, a foaming agent, silicone oil, the heat preservation reinforcing agent prepared in the step (1) and deionized water together, heating to keep the temperature of the whole body at 90-95 ℃, continuously stirring for 2-2.5 h, stopping heating, and naturally cooling to normal temperature.
Further, the wavelength of the ultraviolet ray is controlled to be 300-320 nm during the irradiation treatment in the operation 1) of the step (1), and the irradiation power is 1600-1700W.
Further, the weight volume ratio of the sodium alginate solution, the chitosan solution and the acetic acid-sodium acetate solution in the step (1) and the operation 2) is 4-7 g to 12-15 g: 130-150 ml.
Further, the weight volume ratio of the polycaprolactone, the anhydrous dimethyl sulfoxide and the nano carbon powder in the step (1) operation 3) is 1 g: 12-15 ml: 3-5 g.
Further, in the step (1), the attapulgite, the composite material A and the composite material B in the operation 4) are mixed together, and the corresponding weight-to-volume ratio is 18-22 g: 4-8 g: 90-100 ml.
Further, the viscosity of the plant fiber-based polyether polyol in the step (2) is 2700-2750 mPa · s, and the average functionality is 4-4.5.
Further, the viscosity of the vegetable oil-based polyether polyol in the step (2) is 2800-2850 mPa.s, and the average functionality is 4.5-5.0.
Further, the catalyst in the step (2) is N, N-dimethylcyclohexylamine.
Further, the organic flame retardant in the step (2) is a phosphorus-nitrogen intumescent flame retardant.
Further, the foaming agent in the step (2) is cyclopentane.
The invention has the following beneficial effects:
the invention carries out special improvement treatment on the preparation method of the polyurethane heat-insulating material, in particular to a heat-insulating reinforcing agent component specially prepared on raw materials, the component is processed by taking attapulgite as a matrix, wherein, the attapulgite is firstly subjected to ultraviolet irradiation treatment, the chemical reaction activity on the surface of the attapulgite is enhanced by using the energy of ultraviolet rays, the combination of the attapulgite and the components in subsequent treatment is promoted, then a composite material A and a composite material B are prepared, when the composite material A and the composite material B are mixed and reacted with the attapulgite, the attapulgite can be used as a base point for adhering, fixing and grafting to form a chitosan-sodium alginate-nano carbon powder polymerization-based polyurethane prepolymer macromolecular chain, the chitosan-sodium alginate-nano carbon powder polymerization-based polyurethane prepolymer macromolecular chain has stronger hydrophobicity and heat-insulating capability, has good compatibility and bonding force with the polyurethane matrix, and the heat-insulating reinforcing agent is subsequently combined with diphenylmethane diisocyanate and plant fiber-based polyether polyol, The vegetable oil-based polyether polyol and the like are jointly used for preparing the polyurethane, so that the overall heat insulation performance and stability can be obviously improved, and the overall weight, wear resistance, corrosion resistance and the like of the material can be improved. The method has simple integral steps and is easy to popularize and apply, and the prepared polyurethane thermal insulation material has the characteristics of good thermal insulation, stable use quality, safety, environmental protection and the like, and has great market competitiveness and popularization and application values.
Detailed Description
The following will clearly and completely describe the technical solutions of 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 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
A preparation method of a polyurethane thermal insulation material comprises the following steps:
(1) preparing a heat preservation reinforcing agent:
1) irradiating the attapulgite in an ultraviolet irradiation box for 22min, and taking out for later use;
2) mixing sodium alginate, chitosan and acetic acid-sodium acetate solution, putting into a reaction kettle, continuously stirring for 4h, adding excessive calcium chloride solution into the reaction kettle, continuously stirring for 3h, filtering, washing the filtrate with deionized water to neutrality, and finally drying in a drying oven for 50min to obtain a composite material A for later use;
3) mixing polycaprolactone, anhydrous dimethyl sulfoxide and nano carbon powder, putting into a stirring tank, and stirring and dissolving uniformly to obtain a composite material B for later use;
4) mixing attapulgite treated in the operation 1), the composite material A obtained in the operation 2) and the composite material B obtained in the operation 3) together, putting the mixture into a reaction kettle, filling nitrogen into the reaction kettle, heating to keep the temperature in the reaction kettle at 78 ℃, continuously stirring for 2.5 hours, rapidly cooling the reaction kettle to 20 ℃, adding an excessive ethanol solution into the reaction kettle, filtering, and finally putting the filtrate into a vacuum drying oven for drying for 2 hours and taking out the filtrate to obtain a heat preservation reinforcing agent for later use;
(2) weighing raw materials:
weighing the following raw materials in parts by weight for later use:
70 parts of diphenylmethane diisocyanate, 35 parts of plant fiber-based polyether polyol, 20 parts of plant oil-based polyether polyol, 2 parts of a catalyst, 1 part of an organic flame retardant, 0.5 part of a foaming agent, 1 part of silicone oil, 5 parts of a heat-insulating reinforcing agent prepared in the step (1) and 7 parts of deionized water;
(3) mixing treatment:
mixing diphenylmethane diisocyanate, plant fiber-based polyether polyol and plant oil-based polyether polyol together, adding a catalyst, an organic flame retardant, a foaming agent, silicone oil, the heat preservation reinforcing agent prepared in the step (1) and deionized water together, heating to keep the temperature of the whole body at 90 ℃, continuously stirring for 2 hours, stopping heating, and naturally cooling to normal temperature.
The wavelength of the ultraviolet ray is controlled to be 300nm and the irradiation power is 1600W during the irradiation treatment in the operation 1) of the step (1).
The weight volume ratio of the sodium alginate solution to the chitosan solution to the acetic acid-sodium acetate solution in the step (1) and the operation 2) is 4g to 12 g: 130 ml.
The corresponding weight volume ratio of the polycaprolactone, the anhydrous dimethyl sulfoxide and the nano carbon powder in the step (1) and the operation 3) is 1 g:12 ml: 3g of the total weight.
When the attapulgite, the composite material A and the composite material B in the operation 4) of the step (1) are mixed together, the corresponding weight-to-volume ratio is 18 g: 4g: 90 ml.
The vegetable fibre based polyether polyol described in step (2) has a viscosity of 2700mPa · s and an average functionality of 4.
The vegetable oil-based polyether polyol described in step (2) had a viscosity of 2800 mPa-s and an average functionality of 4.5.
The catalyst in the step (2) is N, N-dimethylcyclohexylamine.
The organic flame retardant in the step (2) is a phosphorus-nitrogen intumescent flame retardant.
The foaming agent in the step (2) is cyclopentane.
Example 2
A preparation method of a polyurethane thermal insulation material comprises the following steps:
(1) preparing a heat preservation reinforcing agent:
1) irradiating the attapulgite in an ultraviolet irradiation box for 25min, and taking out for later use;
2) mixing sodium alginate, chitosan and acetic acid-sodium acetate solution, putting into a reaction kettle, continuously stirring for 5h, adding excessive calcium chloride solution into the reaction kettle, continuously stirring for 4h, filtering, washing the filtrate with deionized water to neutrality, and finally drying in a drying oven for 55min to obtain a composite material A for later use;
3) mixing polycaprolactone, anhydrous dimethyl sulfoxide and nano carbon powder, putting into a stirring tank, and stirring and dissolving uniformly to obtain a composite material B for later use;
4) mixing the attapulgite treated in the operation 1), the composite material A obtained in the operation 2) and the composite material B obtained in the operation 3) together, putting the mixture into a reaction kettle, filling nitrogen into the reaction kettle, heating to keep the temperature in the reaction kettle at 80 ℃, continuously stirring for 3 hours, rapidly cooling the reaction kettle to 22 ℃, adding an excessive ethanol solution into the reaction kettle, filtering, and finally putting the filtrate into a vacuum drying oven for drying for 2.5 hours and taking out the filtrate to obtain a heat preservation reinforcing agent for later use;
(2) weighing raw materials:
weighing the following raw materials in parts by weight for later use:
73 parts of diphenylmethane diisocyanate, 40 parts of plant fiber-based polyether polyol, 30 parts of plant oil-based polyether polyol, 3 parts of a catalyst, 2 parts of an organic flame retardant, 1 part of a foaming agent, 3 parts of silicone oil, 7 parts of a heat-insulating reinforcing agent prepared in the step (1) and 8 parts of deionized water;
(3) mixing treatment:
mixing diphenylmethane diisocyanate, plant fiber-based polyether polyol and plant oil-based polyether polyol together, adding a catalyst, an organic flame retardant, a foaming agent, silicone oil, the heat-insulating reinforcing agent prepared in the step (1) and deionized water together, heating to keep the overall temperature at 93 ℃, continuously stirring for 2.3 hours, stopping heating, and naturally cooling to normal temperature.
The wavelength of ultraviolet rays is controlled to be 310nm during the irradiation treatment in the operation 1) of the step (1), and the irradiation power is 1660W.
The weight volume ratio of the sodium alginate solution to the chitosan solution to the acetic acid-sodium acetate solution in the step (1) and the operation 2) is 6g to 14 g: 140 ml.
The corresponding weight volume ratio of the polycaprolactone, the anhydrous dimethyl sulfoxide and the nano carbon powder in the step (1) and the operation 3) is 1 g:14 ml: 4g of the total weight.
When the attapulgite, the composite material A and the composite material B in the operation 4) of the step (1) are mixed together, the corresponding weight-to-volume ratio is 20 g: 6g: 95 ml.
The viscosity of the plant fiber-based polyether polyol in the step (2) is 2730mPa · s, and the average functionality is 4.2.
The viscosity of the vegetable oil-based polyether polyol in the step (2) is 2840mPa · s, and the average functionality is 4.8.
The catalyst in the step (2) is N, N-dimethylcyclohexylamine.
The organic flame retardant in the step (2) is a phosphorus-nitrogen intumescent flame retardant.
The foaming agent in the step (2) is cyclopentane.
Example 3
A preparation method of a polyurethane thermal insulation material comprises the following steps:
(1) preparing a heat preservation reinforcing agent:
1) irradiating the attapulgite in an ultraviolet irradiation box for 26min, and taking out for later use;
2) mixing sodium alginate, chitosan and acetic acid-sodium acetate solution, putting into a reaction kettle, continuously stirring for 6h, adding excessive calcium chloride solution into the reaction kettle, continuously stirring for 5h, filtering, washing the filtrate with deionized water to neutrality, and finally drying in a drying oven for 60min to obtain a composite material A for later use;
3) mixing polycaprolactone, anhydrous dimethyl sulfoxide and nano carbon powder, putting into a stirring tank, and stirring and dissolving uniformly to obtain a composite material B for later use;
4) mixing attapulgite treated in the operation 1), the composite material A obtained in the operation 2) and the composite material B obtained in the operation 3) together, putting the mixture into a reaction kettle, filling nitrogen into the reaction kettle, heating to keep the temperature in the reaction kettle at 83 ℃, continuously stirring for 3.5 hours, rapidly cooling the reaction kettle to 23 ℃, adding an excessive ethanol solution into the reaction kettle, filtering, and finally putting the filtrate into a vacuum drying oven for drying for 3 hours and taking out the filtrate to obtain a heat preservation reinforcing agent for later use;
(2) weighing raw materials:
weighing the following raw materials in parts by weight for later use:
75 parts of diphenylmethane diisocyanate, 45 parts of plant fiber-based polyether polyol, 35 parts of plant oil-based polyether polyol, 4 parts of a catalyst, 3 parts of an organic flame retardant, 1.5 parts of a foaming agent, 4 parts of silicone oil, 8 parts of a heat-insulating reinforcing agent prepared in the step (1) and 10 parts of deionized water;
(3) mixing treatment:
mixing diphenylmethane diisocyanate, plant fiber-based polyether polyol and plant oil-based polyether polyol together, adding a catalyst, an organic flame retardant, a foaming agent, silicone oil, the heat preservation reinforcing agent prepared in the step (1) and deionized water together, heating to keep the temperature of the whole body at 95 ℃, continuously stirring for 2.5 hours, stopping heating, and naturally cooling to the normal temperature.
Controlling the wavelength of ultraviolet rays to be 320nm and the irradiation power to be 1700W during the irradiation treatment in the operation 1) of the step (1).
The weight volume ratio of the sodium alginate solution to the chitosan solution to the acetic acid-sodium acetate solution in the step (1) and the operation 2) is 7g to 15 g: 150 ml.
The corresponding weight volume ratio of the polycaprolactone, the anhydrous dimethyl sulfoxide and the nano carbon powder in the step (1) and the operation 3) is 1 g:15 ml: 5g of the total weight.
When the attapulgite, the composite material A and the composite material B in the operation 4) of the step (1) are mixed together, the corresponding weight-to-volume ratio is 22 g: 8 g: 100 ml.
The viscosity of the plant fiber-based polyether polyol in step (2) is 2750mPa · s, and the average functionality is 4.5.
The viscosity of the vegetable oil-based polyether polyol in the step (2) is 2850mPa · s, and the average functionality is 5.0.
The catalyst in the step (2) is N, N-dimethylcyclohexylamine.
The organic flame retardant in the step (2) is a phosphorus-nitrogen intumescent flame retardant.
The foaming agent in the step (2) is cyclopentane.
Comparative example 1
The comparative example 1 is different from the example 2 only in that the treatment of the operation 2) is omitted in the preparation of the heat preservation reinforcing agent in the step (1), namely, the addition of the composite material A is omitted, except that the steps of the method are the same.
Comparative example 2
The comparative example 2 is different from the example 2 only in that the nano carbon powder in the operation 3) is not added in the preparation of the heat preservation reinforcing agent in the step (1), except that the steps of the other methods are the same.
Comparative example 3
This comparative example 3 is different from example 2 only in that, in the weighing of the raw material in the step (2), the heat retention enhancer component is replaced with an equal mass part of commercially available ordinary attapulgite, except that the other steps of the method are the same.
Comparative example 4
This comparative example 4 is different from example 2 only in that the heat-insulating reinforcing agent component is omitted in the weighing of the raw material in the step (2), and the steps are the same except for the above.
In order to compare the effects of the invention, the performance tests of the polyurethane thermal insulation materials prepared in the above example 2 and comparative examples 1 to 4 are performed, and the specific comparative data are shown in the following table 1:
TABLE 1
As can be seen from the above table 1, the polyurethane thermal insulation material prepared by the method of the invention has the advantages of obviously improved comprehensive qualities of thermal insulation, strength and the like, obviously improved use value and great market competitiveness.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention, and the present invention is not limited to the illustrated embodiments, and all the modifications and equivalents of the embodiments may be made without departing from the spirit of the present invention.
Claims (10)
1. The preparation method of the polyurethane thermal insulation material is characterized by comprising the following steps:
(1) preparing a heat preservation reinforcing agent:
1) carrying out irradiation treatment on the attapulgite in an ultraviolet irradiation box, and taking out for later use after 22-26 min;
2) mixing sodium alginate, chitosan and acetic acid-sodium acetate solution, putting into a reaction kettle, continuously stirring for 4-6 h, adding excessive calcium chloride solution into the reaction kettle, continuously stirring for 3-5 h, filtering, washing the filtrate with deionized water to neutrality, and finally putting into a drying oven for drying for 50-60 min to obtain a composite material A for later use;
3) mixing polycaprolactone, anhydrous dimethyl sulfoxide and nano carbon powder, putting into a stirring tank, and stirring and dissolving uniformly to obtain a composite material B for later use;
4) mixing attapulgite treated in the operation 1), the composite material A obtained in the operation 2) and the composite material B obtained in the operation 3) together, putting the mixture into a reaction kettle, filling nitrogen into the reaction kettle, heating to keep the temperature in the reaction kettle at 78-83 ℃, continuously stirring for 2.5-3.5 hours, rapidly cooling the reaction kettle to 20-23 ℃, adding an excessive ethanol solution into the reaction kettle, filtering, putting the filtrate into a vacuum drying oven for drying for 2-3 hours, and taking out the filtrate to obtain a heat preservation reinforcing agent for later use;
(2) weighing raw materials:
weighing the following raw materials in parts by weight for later use:
70-75 parts of diphenylmethane diisocyanate, 35-45 parts of plant fiber-based polyether polyol, 20-35 parts of plant oil-based polyether polyol, 2-4 parts of a catalyst, 1-3 parts of an organic flame retardant, 0.5-1.5 parts of a foaming agent, 1-4 parts of silicone oil, 5-8 parts of a heat preservation reinforcing agent prepared in the step (1) and 7-10 parts of deionized water;
(3) mixing treatment:
mixing diphenylmethane diisocyanate, plant fiber-based polyether polyol and plant oil-based polyether polyol together, then adding a catalyst, an organic flame retardant, a foaming agent, silicone oil, the heat preservation reinforcing agent prepared in the step (1) and deionized water together, heating to keep the temperature of the whole body at 90-95 ℃, continuously stirring for 2-2.5 h, stopping heating, and naturally cooling to normal temperature.
2. The preparation method of the polyurethane thermal insulation material as claimed in claim 1, wherein the wavelength of the ultraviolet ray is controlled to be 300-320 nm and the irradiation power is controlled to be 1600-1700W during the irradiation treatment in the operation 1) of the step (1).
3. The preparation method of the polyurethane heat-insulating material as claimed in claim 1, wherein the corresponding weight-to-volume ratio of the sodium alginate, the chitosan and the acetic acid-sodium acetate solution in the step (1) and the operation 2) is 4-7 g: 12-15 g: 130-150 ml.
4. The preparation method of the polyurethane thermal insulation material according to claim 1, wherein the weight volume ratio of the polycaprolactone, the anhydrous dimethyl sulfoxide and the nano carbon powder in the step (1), operation 3) is 1 g: 12-15 ml: 3-5 g.
5. The preparation method of the polyurethane thermal insulation material according to claim 1, wherein the weight volume ratio of the attapulgite, the composite material A and the composite material B in the operation 4) in the step (1) is 18-22 g: 4-8 g: 90-100 ml.
6. The preparation method of the polyurethane thermal insulation material as claimed in claim 1, wherein the viscosity of the plant fiber-based polyether polyol in the step (2) is 2700-2750 mPa-s, and the average functionality is 4-4.5.
7. The method for preparing the polyurethane thermal insulation material as claimed in claim 1, wherein the vegetable oil-based polyether polyol in the step (2) has a viscosity of 2800 to 2850mPa · s and an average functionality of 4.5 to 5.0.
8. The method for preparing polyurethane thermal insulation material according to claim 1, wherein the catalyst in the step (2) is N, N-dimethylcyclohexylamine.
9. The method for preparing polyurethane thermal insulation material according to claim 1, wherein the organic flame retardant in step (2) is a phosphorus-nitrogen intumescent flame retardant.
10. The method for preparing polyurethane thermal insulation material as claimed in claim 1, wherein the blowing agent in step (2) is cyclopentane.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202011187844.3A CN112280287A (en) | 2020-10-29 | 2020-10-29 | Preparation method of polyurethane thermal insulation material |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202011187844.3A CN112280287A (en) | 2020-10-29 | 2020-10-29 | Preparation method of polyurethane thermal insulation material |
Publications (1)
Publication Number | Publication Date |
---|---|
CN112280287A true CN112280287A (en) | 2021-01-29 |
Family
ID=74352926
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN202011187844.3A Pending CN112280287A (en) | 2020-10-29 | 2020-10-29 | Preparation method of polyurethane thermal insulation material |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN112280287A (en) |
Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102786646A (en) * | 2012-08-17 | 2012-11-21 | 江苏大学 | Acid modified palygorskite-polyurethane porous material as well as preparation method and application thereof |
CN103665293A (en) * | 2013-12-12 | 2014-03-26 | 中科院广州能源所盱眙凹土研发中心 | Preparation method of attapulgite modified bio-based polyurethane foam insulation material |
CN106188488A (en) * | 2016-08-03 | 2016-12-07 | 南宁可煜能源科技有限公司 | A kind of polyurethane heat insulation material |
CN106220822A (en) * | 2016-08-25 | 2016-12-14 | 胡国旺 | Polyurethane heat insulation material |
CN109912961A (en) * | 2019-04-04 | 2019-06-21 | 张宏春 | A kind of production method of plastic pipe heat preservation layer material |
CN109912964A (en) * | 2019-04-04 | 2019-06-21 | 张宏春 | A kind of polyurethane insulation coating renovation agent |
-
2020
- 2020-10-29 CN CN202011187844.3A patent/CN112280287A/en active Pending
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102786646A (en) * | 2012-08-17 | 2012-11-21 | 江苏大学 | Acid modified palygorskite-polyurethane porous material as well as preparation method and application thereof |
CN103665293A (en) * | 2013-12-12 | 2014-03-26 | 中科院广州能源所盱眙凹土研发中心 | Preparation method of attapulgite modified bio-based polyurethane foam insulation material |
CN106188488A (en) * | 2016-08-03 | 2016-12-07 | 南宁可煜能源科技有限公司 | A kind of polyurethane heat insulation material |
CN106220822A (en) * | 2016-08-25 | 2016-12-14 | 胡国旺 | Polyurethane heat insulation material |
CN109912961A (en) * | 2019-04-04 | 2019-06-21 | 张宏春 | A kind of production method of plastic pipe heat preservation layer material |
CN109912964A (en) * | 2019-04-04 | 2019-06-21 | 张宏春 | A kind of polyurethane insulation coating renovation agent |
Non-Patent Citations (1)
Title |
---|
张玉龙等: "《纳米技术与纳米塑料》", 31 January 2002, 中国轻工业出版社 * |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN101717514B (en) | Modified phenolic resin, foamed material thereof and method for preparing same | |
CN107779024A (en) | A kind of heat-preservation building paint containing nanoparticle and preparation method thereof | |
CN112694585B (en) | Hard polyisocyanurate node material for insulating deep-sea transmission pipeline interface and preparation method thereof | |
CN105111676A (en) | Preparation method and application of light-weight high-strength plate made of phenolic aldehyde foam composites | |
CN107629186A (en) | A kind of preparation method of resistance combustion polyurethane foam | |
CN112898766A (en) | Hard antibacterial plastic material and preparation method thereof | |
CN110372838B (en) | Combined polyether polyol, polyurethane foam and preparation method thereof | |
CN111269001B (en) | Aerogel composite coiled material produced by halogen-free ammonia-free supercritical process | |
CN112280287A (en) | Preparation method of polyurethane thermal insulation material | |
CN112661925B (en) | Flame-retardant polyurethane foaming thermal insulation material for thermal insulation sandwich board and preparation method thereof | |
CN106046766B (en) | A kind of automobile plastic high intensity modified nylon materials | |
CN112812714A (en) | Fireproof flame-retardant buffer aerogel product capable of absorbing stress and manufacturing method thereof | |
CN108129689A (en) | The preparation process of the shockproof polyurethane foam of heat conduction | |
CN112358647A (en) | High-strength polyurethane rigid foam plastic and preparation method thereof | |
CN109867942B (en) | Preparation method of flame-retardant micro-foaming polyphenyl ether composite material and product thereof | |
CN106995565A (en) | A kind of preparation method of the sol-gel modified poly styrene composite material of fire-retardant phosphotidic | |
CN107739168B (en) | Flame-retardant thermal-insulation material containing expanded vermiculite with low thermal conductivity coefficient and preparation method thereof | |
CN109021461B (en) | Preparation method of environment-friendly interior wall decorative plate | |
CN114195975A (en) | High-flame-retardance low-temperature foaming type broken bridge aluminum door and window penetrating strip foaming material combined polyether and preparation method thereof, polyurethane foam and preparation method thereof | |
CN106928648B (en) | Whisker reinforced toughened halogen-free flame-retardant phenolic foam plastic and preparation method thereof | |
CN115260598A (en) | High-strength aerogel for heat insulation material and preparation method thereof | |
CN114106503A (en) | High-strength expandable polystyrene filling resin and preparation method thereof | |
CN111777734A (en) | Flame-retardant polyether material for polyurethane foaming product | |
CN110272587B (en) | Cold-resistant high-temperature-resistant flame-retardant composite material and preparation method thereof | |
CN112280290A (en) | Flame-retardant polyurethane rigid foam and preparation method thereof |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
RJ01 | Rejection of invention patent application after publication | ||
RJ01 | Rejection of invention patent application after publication |
Application publication date: 20210129 |