Thermal insulation material and finished product crystallization reaction kettle applied to intermediate synthesis

Abstract

The invention relates to a thermal insulation material and a finished product crystallization reaction kettle applied to intermediate synthesis, and belongs to the technical field of thermal insulation materials. The preparation method comprises the following steps: carrying out ring opening on vinyl ethylene oxide through diluted hydrochloric acid to obtain 4-chloro-1-butene-3-alcohol, reacting with paratoluensulfonyl chloride to obtain a sulfonate derivative, reacting with magnesium chips to generate a Grignard reagent, and reacting with tetraethoxysilane to obtain sulfonate silane; then, sulfonate silane and sodium azide are subjected to an azido reaction to obtain azido silane, and azido silane and triphenylphosphine are subjected to a reaction and purification to obtain an amino co-precursor; mixing and reacting the amino co-precursor with tetraethoxysilane, absolute ethyl alcohol and deionized water, and aging and drying to obtain hydrophobic amino silicon dioxide aerogel; and finally, taking polyether polyol as a base material, adding the hydrophobic amino silicon dioxide aerogel, and reacting with diphenylmethane diisocyanate to obtain the thermal insulation material.

Description

Technical Field

[0001] This invention belongs to the field of thermal insulation materials technology, specifically, it relates to a thermal insulation material and its application in the crystallization reactor for intermediate synthesis. Background Technology

[0002] Rigid polyurethane foam, with its extremely low thermal conductivity, can effectively block heat transfer, providing core protection for thermal insulation. It also possesses excellent mechanical properties, allowing it to withstand certain external forces without easily being damaged. Combined with its outstanding aging resistance and chemical resistance, it maintains stable performance even in long-term outdoor environments or exposure to corrosive substances. Therefore, it is not only widely used in building exterior walls and roofs to reduce building energy consumption, but also serves as a key insulation material for heating pipes and industrial equipment, effectively improving the energy efficiency and lifespan of various facilities.

[0003] Silica aerogel (SA) is highly valued for its lightweight, high porosity, high specific surface area, and low thermal conductivity, making it ideal for thermal insulation applications. However, SA's surface is rich in hydroxyl groups, resulting in high surface energy and a tendency to aggregate. Furthermore, the strong polarity of the silanol groups allows them to bind with water molecules through hydrogen bonds, leading to the aerogel absorbing moisture from the environment. Since moisture has a much higher thermal conductivity than air, this process disrupts the aerogel's porous insulating structure, ultimately causing a significant decrease in its insulation performance and inhibiting the expression of its superior properties. Therefore, surface modification of nano-SA is a necessary prerequisite for preparing composite insulation materials with excellent thermal insulation and thermodynamic properties. Summary of the Invention

[0004] The purpose of this invention is to provide a thermal insulation material and a finished crystallization reactor for intermediate synthesis, in order to solve the problems mentioned in the background art.

[0005] The objective of this invention can be achieved through the following technical solutions: A method for preparing a heat-insulating material for a reaction vessel includes the following steps: The hydrophobic amino silica aerogel was mixed with the polyether polyol, and then diphenylmethane diisocyanate, triethanolamine, pentafluorobutane, and silicone oil were added. The mixture was stirred with an electric stirrer at 2800–3000 r·min. -1 Mix and stir at high speed for 3-6 minutes, then foam at 40-45℃ for 10-15 minutes. After curing and cooling, the insulation material is obtained.

[0006] Furthermore, the hydrophobic amino silica aerogel is obtained by the condensation reaction of tetraethyl orthosilicate and an amino co-precursor, and the hydrophobic amino silica aerogel can be prepared by the following methods: First, tetraethyl orthosilicate and amino co-precursor are mixed evenly. Then, anhydrous ethanol, deionized water, dilute hydrochloric acid and N,N-dimethylformamide are added. The mixture is stirred and reacted at 50-55℃ for 8-12 hours. After aging and drying, hydrophobic amino silica aerogel is obtained.

[0007] Furthermore, the amino co-precursor is prepared by the following steps: S1. Dilute hydrochloric acid was added to vinyl ethylene oxide and stirred at room temperature. After the reaction was completed, the organic phase was extracted with ethyl acetate and separated. Then, the organic phase was washed successively with saturated sodium bicarbonate aqueous solution and saturated brine, dried, and the ethyl acetate was removed by rotary evaporation to obtain 4-chloro-1-buten-3-ol.

[0008] S2. Add 4-chloro-1-buten-3-ol to pyridine, then add p-toluenesulfonyl chloride, and stir the reaction at 0-5℃ for 3-5 h. After the reaction is completed, pour the reaction solution into ice water, then extract with diethyl ether to separate the organic phase, then wash with saturated sodium bicarbonate aqueous solution and saturated brine in sequence, then dry, and finally remove the solvent by vacuum distillation to obtain the sulfonate derivative.

[0009] S3. Under a nitrogen atmosphere, magnesium shavings and tetraethyl orthosilicate are added to anhydrous tetrahydrofuran and stirred. Then, the sulfonate derivative is added and refluxed at 70-75°C for 12-16 hours. After cooling to room temperature, the solid is removed by filtration, the tetrahydrofuran is removed by rotary evaporation, and the fraction is collected by vacuum distillation to obtain sulfonate silane.

[0010] S4. Dissolve sulfonate silane and sodium azide in N,N-dimethylformamide and stir at 80-85°C for 24-30 h. After the reaction is completed, cool to room temperature and pour the reaction solution into ice water. Extract with ethyl acetate to separate the organic phase. Wash with deionized water and saturated brine in sequence, dry, and finally remove ethyl acetate by vacuum distillation to obtain azide silane.

[0011] S5. Dissolve azidosilane in tetrahydrofuran, then add triphenylphosphine and deionized water, stir and mix well for 18-20 h. After the reaction is complete, pour the reaction solution into water, extract with ethyl acetate, separate the organic phase and wash with saturated brine, dry, and finally remove ethyl acetate by vacuum distillation and separate the product by column chromatography to obtain the amino co-precursor.

[0012] Furthermore, in the preparation method of hydrophobic amino silica aerogel, the mass ratio of hydrophobic amino silica aerogel, polyether polyol, diphenylmethane diisocyanate, triethanolamine, pentafluorobutane, and silicone oil is 5-8:80-100:100-125:0.3-0.4:1.3-1.7:1.6-2.

[0013] Furthermore, the polyether polyol is at least one of polytetrahydrofuran ether diol and polyethylene glycol.

[0014] Furthermore, in the preparation method of hydrophobic amino silica aerogel, the mass ratio of tetraethyl orthosilicate, amino co-precursor, anhydrous ethanol, deionized water, dilute hydrochloric acid, and N,N-dimethylformamide is 38-40:10-12:65-75:20-26:1-3:8-10.

[0015] Furthermore, the mass fraction of the dilute hydrochloric acid is 5% to 10%.

[0016] Furthermore, the mass ratio of vinyl ethylene oxide to dilute hydrochloric acid in S1 is 70-75:400-450.

[0017] Furthermore, the mass ratio of 4-chloro-1-buten-3-ol, pyridine, and p-toluenesulfonyl chloride in S2 is 50–55: 75–85: 90–100.

[0018] Furthermore, the mass ratio of sulfonate derivatives, magnesium shavings, and tetraethyl orthosilicate in S3 is 38–40: 5–6.5: 20–26.

[0019] Furthermore, the mass ratio of sulfonate silane to sodium azide in S4 is 25–30:5–6.5.

[0020] Furthermore, the mass ratio of azidosilane, triphenylphosphine, and deionized water in S5 is 15–20:34–45:3.6–5.8.

[0021] Furthermore, the insulation material is applied to the crystallization reactor for the intermediate synthesis.

[0022] The beneficial effects of this invention are: 1) In this invention, 4-chloro-1-buten-3-ol is obtained by ring-opening vinyl ethylene oxide with dilute hydrochloric acid, which is then reacted with p-toluenesulfonyl chloride to obtain a sulfonate derivative. Subsequently, it is reacted with magnesium filings to generate a Grignard reagent, which is then reacted with tetraethyl orthosilicate to obtain a sulfonate silane. The sulfonate silane is then subjected to an azide reaction with sodium azide to obtain azide silane, which is then purified by reacting with triphenylphosphine to obtain an amino co-precursor. The amino co-precursor, tetraethyl orthosilicate, anhydrous ethanol, and deionized water are then mixed and reacted, followed by aging and drying to obtain a hydrophobic amino silica aerogel. Finally, a polyether polyol is used as a base material, and the hydrophobic amino silica aerogel is added, which is then reacted with diphenylmethane diisocyanate to obtain a thermal insulation material.

[0023] 2) This invention utilizes chemical grafting to graft nonpolar segments onto the porous framework surface of aerogel, covering polar hydroxyl groups and reducing surface energy. The segments contain only C-C single bonds, C=C double bonds, and CH bonds, with no polar bonds, making the molecules as a whole nonpolar and repelling polar water molecules, thereby achieving a hydrophobic effect and ensuring the stability of the thermal insulation performance of silica aerogel.

[0024] 3) This invention introduces amino groups on the surface of the aerogel. As a highly polar active group, the amino group can react with the groups in the polyurethane molecular chain to form a tighter chemical bonding interface, which significantly improves the dispersion uniformity of the aerogel in the polyurethane matrix, avoids problems such as agglomeration, and improves the overall mechanical properties and thermal insulation capacity of the composite material. Detailed Implementation

[0025] The technical solutions of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of the present invention.

[0026] The room temperature was 25±5℃.

[0027] Example 1

[0028] A method for preparing a heat-insulating material for a reaction vessel includes the following steps: By weight, 5 parts of hydrophobic amino silica aerogel were mixed with 100 parts of polytetrahydrofuran ether glycol, and then 100 parts of diphenylmethane diisocyanate, 0.4 parts of triethanolamine, 1.7 parts of pentafluorobutane, and 1.6 parts of silicone oil were added. The mixture was stirred using an electric stirrer at 2800 r·min. -1 Mix and stir at high speed for 6 minutes, foam at 45°C for 10 minutes, then mature at 80°C for 12 hours, and finally place at room temperature to obtain the thermal insulation material.

[0029] The preparation method of the hydrophobic amino silica aerogel is as follows: By mass fraction, 40 parts of tetraethyl orthosilicate and 10 parts of amino co-precursor were mixed evenly, and then 75 parts of anhydrous ethanol, 20 parts of deionized water, 3 parts of 5% dilute hydrochloric acid and 10 parts of N,N-dimethylformamide were added. The mixture was stirred at 50°C for 12 hours, and after aging and drying, hydrophobic amino silica aerogel was obtained.

[0030] The amino co-precursor is prepared by the following steps: S1. By mass, 70 parts of vinyl ethylene oxide were added to 450 parts of dilute hydrochloric acid and stirred at room temperature. After the reaction was completed, the organic phase was extracted with ethyl acetate and separated. Then, the organic phase was washed successively with saturated sodium bicarbonate aqueous solution and saturated brine, dried, and the ethyl acetate was removed by rotary evaporation. The purified product was 4-chloro-1-buten-3-ol.

[0031] S2. By mass, 53 parts of 4-chloro-1-buten-3-ol were added to 80 parts of pyridine, followed by 100 parts of p-toluenesulfonyl chloride. The mixture was stirred at 5°C for 3 hours. After the reaction was completed, the reaction solution was poured into ice water and extracted with diethyl ether to separate the organic phase. The solution was then washed successively with dilute hydrochloric acid, saturated sodium bicarbonate aqueous solution, and saturated brine, dried, and finally the solvent was removed by vacuum distillation to obtain the sulfonate derivative.

[0032] S3. By mass, under a nitrogen atmosphere, 5.8 parts of magnesium shavings and 23 parts of tetraethyl orthosilicate were added to anhydrous tetrahydrofuran and stirred. Then, 39 parts of sulfonate derivative were added and refluxed at 73°C for 14 hours. After cooling to room temperature, the solid was removed by filtration, the tetrahydrofuran was removed by rotary evaporation, and the fraction was collected by vacuum distillation to obtain sulfonate silane.

[0033] S4. By mass fraction, 25 parts of sulfonate silane and 6.5 parts of sodium azide were dissolved in N,N-dimethylformamide and stirred at 80°C for 30 h. After the reaction was completed, the mixture was cooled to room temperature and poured into ice water. The mixture was then extracted with ethyl acetate to separate the organic phase. The organic phase was washed successively with deionized water and saturated brine, dried, and finally removed by vacuum distillation to obtain azidosilane.

[0034] S5. Dissolve 15 parts of azidosilane in tetrahydrofuran by mass, then add 45 parts of triphenylphosphine and 3.6 parts of deionized water, stir and mix well for 20 h. After the reaction is completed, pour the reaction solution into water, then extract with ethyl acetate, separate the organic phase and wash with saturated brine, dry, and finally remove ethyl acetate by vacuum distillation and separate the product by column chromatography to obtain the amino co-precursor.

[0035] Example 2

[0036] A method for preparing a heat-insulating material for a reaction vessel includes the following steps: By weight, 8 parts of hydrophobic amino silica aerogel were mixed with 80 parts of polyethylene glycol, and then 125 parts of diphenylmethane diisocyanate, 0.3 parts of triethanolamine, 1.3 parts of pentafluorobutane, and 2 parts of silicone oil were added. The mixture was stirred using an electric stirrer at 3000 r·min. -1 Mix and stir at high speed for 3 minutes, foam at 40°C for 15 minutes, then mature at 85°C for 24 hours, and finally place at room temperature to obtain the thermal insulation material.

[0037] The preparation method of the hydrophobic amino silica aerogel is as follows: By mass fraction, 38 parts of tetraethyl orthosilicate and 12 parts of amino co-precursor were first mixed evenly, and then 65 parts of anhydrous ethanol, 26 parts of deionized water, 1 part of 10% dilute hydrochloric acid and 8 parts of N,N-dimethylformamide were added. The mixture was stirred and reacted at 55°C for 8 hours. After aging and drying, hydrophobic amino silica aerogel was obtained.

[0038] The amino co-precursor is prepared by the following steps: S1. By mass, 73 parts of vinyl ethylene oxide were added to 425 parts of dilute hydrochloric acid and stirred at room temperature. After the reaction was completed, the organic phase was extracted with ethyl acetate and separated. Then, the organic phase was washed successively with saturated sodium bicarbonate aqueous solution and saturated brine, dried, and the ethyl acetate was removed by rotary evaporation. The purified product was 4-chloro-1-buten-3-ol.

[0039] S2. By mass, add 50 parts of 4-chloro-1-buten-3-ol to 85 parts of pyridine, then add 90 parts of p-toluenesulfonyl chloride, stir the reaction at 0℃ for 5 h. After the reaction is completed, pour the reaction solution into ice water, then extract with diethyl ether to separate the organic phase, then wash with dilute hydrochloric acid, saturated sodium bicarbonate aqueous solution and saturated brine in sequence, then dry, and finally remove the solvent by vacuum distillation to obtain the sulfonate derivative.

[0040] S3. By mass, under a nitrogen atmosphere, add 5 parts magnesium shavings and 26 parts tetraethyl orthosilicate to anhydrous tetrahydrofuran, stir, then add 38 parts sulfonate derivative, reflux at 75°C for 12 h, cool to room temperature, filter to remove solid, remove tetrahydrofuran by rotary evaporation, and then collect the fraction by vacuum distillation to obtain sulfonate silane.

[0041] S4. By mass fraction, 30 parts of sulfonate silane and 5 parts of sodium azide are dissolved in N,N-dimethylformamide and stirred at 85°C for 24 h. After the reaction is completed, the mixture is cooled to room temperature and poured into ice water. The mixture is then extracted with ethyl acetate to separate the organic phase. The organic phase is washed successively with deionized water and saturated brine, dried, and finally removed by vacuum distillation to obtain azidosilane.

[0042] S5. By mass, 20 parts of azidosilane were dissolved in tetrahydrofuran, and then 34 parts of triphenylphosphine and 5.8 parts of deionized water were added. The mixture was stirred and stirred for 18 hours. After the reaction was completed, the reaction solution was poured into water and then extracted with ethyl acetate. The organic phase was separated and washed with saturated brine. The solution was then dried and the ethyl acetate was removed by vacuum distillation. The residue was separated by column chromatography to obtain the amino co-precursor.

[0043] Example 3

[0044] A method for preparing a heat-insulating material for a reaction vessel includes the following steps: By weight, 6 parts of hydrophobic amino silica aerogel were mixed with 90 parts of polytetrahydrofuran ether glycol, and then 110 parts of diphenylmethane diisocyanate, 0.38 parts of triethanolamine, 1.5 parts of pentafluorobutane, and 1.8 parts of silicone oil were added. The mixture was stirred using an electric stirrer at 2900 r·min. -1 Mix and stir at high speed for 5 minutes, foam at 43°C for 13 minutes, then mature at 82°C for 20 hours, and finally place at room temperature to obtain the thermal insulation material.

[0045] The preparation method of the hydrophobic amino silica aerogel is as follows: By mass fraction, 39 parts of tetraethyl orthosilicate and 11 parts of amino co-precursor were first mixed evenly, and then 70 parts of anhydrous ethanol, 23 parts of deionized water, 2 parts of dilute hydrochloric acid with a mass fraction of 8% and 9 parts of N,N-dimethylformamide were added. The mixture was stirred and reacted at 53°C for 10 hours. After aging and drying, hydrophobic amino silica aerogel was obtained.

[0046] The amino co-precursor is prepared by the following steps: S1. By mass, 70 parts of vinyl ethylene oxide were added to 400 parts of dilute hydrochloric acid and stirred at room temperature. After the reaction was completed, the organic phase was extracted with ethyl acetate and separated. Then, the organic phase was washed successively with saturated sodium bicarbonate aqueous solution and saturated brine, dried, and the ethyl acetate was removed by rotary evaporation to obtain 4-chloro-1-buten-3-ol.

[0047] S2. By mass, 55 parts of 4-chloro-1-buten-3-ol were added to 75 parts of pyridine, followed by 95 parts of p-toluenesulfonyl chloride. The mixture was stirred at 3°C ​​for 4 hours. After the reaction was completed, the reaction solution was poured into ice water and extracted with diethyl ether to separate the organic phase. The solution was then washed successively with dilute hydrochloric acid, saturated sodium bicarbonate aqueous solution, and saturated brine, dried, and finally the solvent was removed by vacuum distillation to obtain the sulfonate derivative.

[0048] S3. By mass, under a nitrogen atmosphere, 6.5 parts magnesium shavings and 20 parts tetraethyl orthosilicate were added to anhydrous tetrahydrofuran and stirred. Then, 40 parts sulfonate derivatives were added and refluxed at 70°C for 16 hours. After cooling to room temperature, the solid was removed by filtration, the tetrahydrofuran was removed by rotary evaporation, and the fraction was collected by vacuum distillation to obtain sulfonate silane.

[0049] S4. By mass fraction, 28 parts of sulfonate silane and 6 parts of sodium azide were dissolved in N,N-dimethylformamide and stirred at 83°C for 28 h. After the reaction was completed, the mixture was cooled to room temperature and poured into ice water. The mixture was then extracted with ethyl acetate to separate the organic phase. The organic phase was washed successively with deionized water and saturated brine, dried, and finally removed by vacuum distillation to obtain azidosilane.

[0050] S5. Dissolve 18 parts by mass of azidosilane in tetrahydrofuran, then add 40 parts of triphenylphosphine and 4.5 parts of deionized water, stir and mix well for 19 h. After the reaction is complete, pour the reaction solution into water, then extract with ethyl acetate, separate the organic phase and wash with saturated brine, dry, and finally remove ethyl acetate by vacuum distillation and separate the product by column chromatography to obtain the amino co-precursor.

[0051] Comparative Example 1 The difference between this comparative example and Example 1 is that the silica aerogel is not modified, while the other raw materials and preparation steps remain unchanged.

[0052] Experimental Example 1 The thermal insulation materials in Examples 1-3 and Comparative Example 1 were subjected to the following performance tests, and the test results are shown in Table 1.

[0053] Water contact angle test: The surface water contact angle of each group of materials was tested in accordance with GB / T30693-2014 "Measurement of water contact angle of plastic film".

[0054] Thermal conductivity test: The test was conducted at an average temperature of 25℃, in accordance with GB / T10295-2019 "Determination of steady-state thermal resistance and related properties of thermal insulation materials by heat flow meter method".

[0055] Compression performance test: The test was conducted in accordance with GB / T8813-2022 "Determination of compression performance of rigid foamed plastics".

[0056] Table 1

[0057] As can be seen from Table 1, the hydrophobic amino silica aerogel added in this invention reduces the thermal conductivity of polyurethane and improves its thermal insulation performance; at the same time, the modified aerogel has improved hydrophobic strength and enhanced compatibility with polyurethane materials, thereby improving the material strength.

[0058] The present invention provides a detailed description of a heat-insulating material for a reaction vessel and its preparation method. Specific examples have been used to illustrate the principles and implementation methods of the invention. The descriptions of these embodiments are merely for the purpose of helping to understand the method and core ideas of the invention, including the best mode, and also to enable any person skilled in the art to practice the invention, including manufacturing and using any device or system, and implementing any combination method. It should be noted that those skilled in the art can make various improvements and modifications to the invention without departing from its principles. In particular, as long as there is no structural conflict, the features in the embodiments disclosed in this invention can be combined with each other in any way. The lack of an exhaustive description of these combinations in this specification is merely for the sake of brevity and resource conservation. Therefore, the present invention is not limited to the specific embodiments disclosed herein, but includes all technical solutions falling within the scope of the claims.

Claims

1. An insulating material, characterized in that, The preparation method of the thermal insulation material is as follows: The hydrophobic aminosilica aerogel and polyether polyol are uniformly mixed, then diphenylmethane diisocyanate, triethanolamine, pentafluorobutane and silicone oil are added, and the thermal insulation material is obtained after foaming reaction; The preparation method of the hydrophobic aminosilica aerogel is as follows: The tetraethyl orthosilicate and amino co-precursor are mixed, then anhydrous ethanol, deionized water, dilute hydrochloric acid and N, N-dimethylformamide are added, and the hydrophobic aminosilica aerogel is obtained after condensation reaction. The preparation method of the amino co-precursor is as follows: S1, the vinyl oxirane is reacted with dilute hydrochloric acid to obtain 4-chloro-1-butene-3-ol; S2, the 4-chloro-1-butene-3-ol is reacted with p-toluenesulfonyl chloride to obtain a sulfonate derivative; S3, the sulfonate derivative is reacted with magnesium and tetraethyl orthosilicate to obtain a sulfonate silane; S4, the sulfonate silane is reacted with sodium azide to obtain an azidosilane; S5, the azidosilane is reacted with triphenylphosphine and deionized water to obtain an amino co-precursor.

2. A thermal insulation material according to claim 1, characterised in that The mass fraction of the dilute hydrochloric acid is 5% to 10%.

3. A thermal insulation material according to claim 1, characterized in that In the preparation method of the thermal insulation material, the mass fraction ratio of the hydrophobic aminosilica aerogel, polyether polyol, diphenylmethane diisocyanate, triethanolamine, pentafluorobutane and silicone oil is 5 to 8:80 to 100:100 to 125:0.3 to 0.4:1.3 to 1.7:1.6 to 2.

4. A thermal insulation material according to claim 1, characterized in that In the preparation method of the hydrophobic aminosilica aerogel, the mass fraction ratio of the tetraethyl orthosilicate, amino co-precursor, anhydrous ethanol, dilute hydrochloric acid, deionized water and N, N-dimethylformamide is 38 to 40:10 to 12:65 to 75:20 to 26:1 to 3:8 to 10.

5. A thermal insulation material according to claim 1, characterized in that In the preparation method of the amino co-precursor, the mass fraction ratio of the vinyl oxirane and dilute hydrochloric acid in S1 is 70 to 75:400 to 450.

6. A thermal insulation material according to claim 1, characterized in that In the preparation method of the amino co-precursor, the mass fraction ratio of the 4-chloro-1-butene-3-ol, pyridine and p-toluenesulfonyl chloride in S2 is 50 to 55:75 to 85:90 to 100.

7. A thermal insulation material according to claim 1, characterized in that In the preparation method of the amino co-precursor, the mass fraction ratio of the sulfonate derivative, magnesium and tetraethyl orthosilicate in S3 is 38 to 40:5 to 6.5:20 to 26.

8. A thermal insulation material according to claim 1, characterized in that In the preparation method of the amino co-precursor, the mass fraction ratio of the sulfonate silane and sodium azide in S4 is 25 to 30:5 to 6.5, and the mass fraction ratio of the azidosilane, triphenylphosphine and deionized water in S5 is 15 to 20:34 to 45:3.6 to 5.

8.

9. A thermal insulation material according to claim 1, characterized in that In the preparation method of the amino co-precursor, the foaming reaction is carried out at 40 to 45℃ for 10 to 15 minutes.

10. Use of an insulating material, characterized in that The thermal insulation material of any one of claims 1 to 9 is applied to a finished product crystallization reaction kettle for intermediate synthesis.

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