CN114957585A - Formula of high-compressive-strength transparent organic material and preparation method thereof - Google Patents

Formula of high-compressive-strength transparent organic material and preparation method thereof Download PDF

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Publication number
CN114957585A
CN114957585A CN202210785403.6A CN202210785403A CN114957585A CN 114957585 A CN114957585 A CN 114957585A CN 202210785403 A CN202210785403 A CN 202210785403A CN 114957585 A CN114957585 A CN 114957585A
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China
Prior art keywords
transparent organic
organic material
compressive strength
heating
chain extender
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CN202210785403.6A
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Chinese (zh)
Inventor
吴贲华
袁厚呈
冯飞
孙钰晶
张鹏
王健
邹海民
张钰柯
张锡祥
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Jiangsu Tiemao Glass Co Ltd
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Jiangsu Tiemao Glass Co Ltd
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Priority to CN202210785403.6A priority Critical patent/CN114957585A/en
Publication of CN114957585A publication Critical patent/CN114957585A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00Polymeric products of isocyanates or isothiocyanates
    • C08G18/06Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/30Low-molecular-weight compounds
    • C08G18/32Polyhydroxy compounds; Polyamines; Hydroxyamines
    • C08G18/3203Polyhydroxy compounds
    • C08G18/3206Polyhydroxy compounds aliphatic
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00Polymeric products of isocyanates or isothiocyanates
    • C08G18/06Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/70Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
    • C08G18/72Polyisocyanates or polyisothiocyanates
    • C08G18/74Polyisocyanates or polyisothiocyanates cyclic
    • C08G18/75Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic
    • C08G18/751Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring
    • C08G18/752Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group
    • C08G18/753Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group
    • C08G18/755Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group and at least one isocyanate or isothiocyanate group linked to a secondary carbon atom of the cycloaliphatic ring, e.g. isophorone diisocyanate
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00Use of organic ingredients
    • C08K5/04Oxygen-containing compounds
    • C08K5/13Phenols; Phenolates
    • C08K5/134Phenols containing ester groups
    • C08K5/1345Carboxylic esters of phenolcarboxylic acids
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00Use of organic ingredients
    • C08K5/16Nitrogen-containing compounds
    • C08K5/34Heterocyclic compounds having nitrogen in the ring
    • C08K5/3467Heterocyclic compounds having nitrogen in the ring having more than two nitrogen atoms in the ring
    • C08K5/3472Five-membered rings
    • C08K5/3475Five-membered rings condensed with carbocyclic rings

Abstract

The application relates to a formula of a high-compressive-strength transparent organic material and a preparation method thereof. The formula comprises the following components in percentage by weight: 75-80% of isocyanate; 5-10% of micromolecular chain extender; 10-15% of a cross-linking agent; 0.5% of antioxidant. The preparation method comprises the following steps: weighing the raw materials according to the formula; dehydrating the micromolecular chain extender in vacuum; uniformly mixing isocyanate and the dehydrated micromolecule chain extender, and heating and stirring to obtain a first material; mixing the cross-linking agent, the antioxidant and the ultraviolet additive, and heating and stirring to obtain a second material; mixing the second material with the first material, and heating and stirring to obtain a castable; pouring the casting material into a mold, curing at high temperature in stages, and removing the mold to obtain the high-compression-strength transparent organic material which is suitable for some special fields and fills the vacancy of the high-compression-strength transparent organic material.

Description

Formula of high-compressive-strength transparent organic material and preparation method thereof
Technical Field
The application relates to a transparent organic material, in particular to a formula of a high-compression-strength transparent organic material and a preparation method thereof.
Background
The transparent organic material is usually polycarbonate and polymethyl methacrylate, and the compression strength of the two materials is about 100Mpa, so that the two materials cannot be used in some special fields. Therefore, it is necessary to design a transparent organic glass with high compressive strength to fill the gap of the transparent organic material with high compressive strength.
Disclosure of Invention
The embodiment of the application provides a formula of a high-compression-strength transparent organic material and a preparation method thereof, and aims to solve the problem that the existing transparent organic material is low in strength.
In order to solve the above technical problem, the present application is implemented as follows:
in a first aspect, a formulation of a compressive strength transparent organic material is provided, which comprises the following components in percentage by weight: 75-80% of isocyanate; 5-10% of micromolecular chain extender; 10-15% of a cross-linking agent; 0.5% of antioxidant; 0.5% of an ultraviolet additive.
In a first possible implementation of the first aspect, the isocyanate comprises one or more of dicyclohexylmethane diisocyanate, p-phenylene diisocyanate, isophorone diisocyanate, 1, 5-naphthalene diisocyanate.
In a second possible implementation of the first aspect, the small molecule chain extender comprises one or more of ethylene glycol, propylene glycol, 1, 4-butanediol, diethylene glycol, 1, 3-butanediol, 1, 5-pentanediol, 2-dimethyl-1, 3-propanediol, methyl propanediol, or diethylene glycol (diethylene glycol).
In a third possible implementation form of the first aspect, the cross-linking agent comprises one or more of glycerol, trimethylolethane, trimethylolpropane, MOCA, diisopropanolamine.
In a fourth possible implementation of the first aspect, the antioxidant is antioxidant 1010 and the ultraviolet additive is UV-328.
In a second aspect, there is provided a method for preparing a high compressive strength transparent organic material, comprising the steps of: (a) weighing the raw materials according to the formula of the transparent organic material with high compressive strength in any one of the first aspect; (b) dehydrating the micromolecule chain extender in vacuum to ensure that the mass fraction of water is less than or equal to 0.05 percent; (c) uniformly mixing isocyanate and the dehydrated micromolecule chain extender, and heating and stirring to obtain a first material; (d) mixing the cross-linking agent, the antioxidant and the ultraviolet additive, and heating and stirring to obtain a second material; (e) mixing the second material with the first material, and heating and stirring to obtain a castable; (f) pouring the casting material into a mold, curing at high temperature in stages, and removing the mold to obtain the high-compression-strength transparent organic material.
In a first possible implementation manner of the second aspect, in the step (b), during the vacuum dehydration of the small molecule chain extender, the small molecule chain extender is added into a three-neck flask equipped with a stirrer and a thermometer, heated to 110 ℃, dehydrated for 2-3h under vacuum, and cooled to 80 ℃ for standby.
In a second possible implementation manner of the second aspect, in the steps (c) to (e), the heating stirring temperature is 80 ℃.
In a third possible implementation manner of the second aspect, in the step (e), after the heating and stirring of the second material and the first material, the second material is further subjected to vacuum degassing.
In a fourth possible implementation manner of the second aspect, in the step (f), during the step of high-temperature stage curing, the curing is performed in stages by heating at 80 ℃ for 2 hours, heating at 115 ℃ for 2 hours, heating at 160 ℃ for 26 hours.
Compared with the prior art, the application has the advantages that:
according to the formula and the preparation method of the high-compressive-strength transparent organic material, compared with the existing transparent organic material, the prepared high-compressive-strength transparent organic material can greatly improve the compressive strength, so that the high-compressive-strength transparent organic material is suitable for some special fields, and the vacancy of the high-compressive-strength transparent organic material is filled. Meanwhile, the preparation method is simple and easy to operate.
Drawings
The accompanying drawings, which are included to provide a further understanding of the application and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the application and together with the description serve to explain the application and not to limit the application. In the drawings:
fig. 1 is a flow chart illustrating steps of a method for preparing a high compressive strength transparent organic material according to an embodiment of the present application.
Detailed Description
To make the objects, technical solutions and advantages of the present application more clear, embodiments of the present application will be described in further detail below with reference to the accompanying drawings.
Example 1
Weighing the following components in percentage by weight: 75% isocyanate (IPDI); 9% of 1, 4-butanediol; 15% trimethylolpropane; 0.5% of antioxidant; 0.5% of an ultraviolet additive.
Please refer to fig. 1, which is a flowchart illustrating a method for preparing a high compressive strength transparent organic material according to an embodiment of the present application. The high compressive strength transparent organic material was prepared according to the above formulation, and the preparation method 1 of the high compressive strength transparent organic material includes the following steps S1 to S6. Wherein:
in step S1, the small molecule chain extender is dehydrated in vacuum so that the mass fraction of water is 0.05% or less. Specifically, 1, 4-butanediol is added into a three-neck flask provided with a stirrer and a thermometer, the mixture is heated to 110 ℃, dehydrated for 2-3h under vacuum, the mass fraction of water in the mixture is not higher than 0.05 percent, and cooled to 80 ℃ for later use.
In step S2, isocyanate and the dehydrated small molecule chain extender are uniformly mixed, heated and stirred to obtain a first material. Specifically, the 1, 4-butanediol dehydrated in the step S1 is added into the metered IPDI, the temperature is kept at 80 ℃, the heating and stirring reaction is carried out for 2-3h, and after the theoretical NCO content is reached, the first material is obtained for standby.
In step S3, the crosslinking agent, the antioxidant, and the ultraviolet additive are mixed, heated, and stirred to obtain a second material. Specifically, trimethylolpropane, antioxidant 1010 and UV-328 are added into a beaker, and stirred at 80 ℃ until the materials are melted, so that a second material is obtained for later use.
In step S4, the second material and the first material are mixed, heated and stirred to obtain the castable. Specifically, the second material is added into a three-neck flask of the first material, the first material and the second material are stirred by a stirrer in the three-neck flask at 80 ℃ until the materials are clear, and then bubbles are removed in vacuum for 5 minutes to obtain the castable.
In step S5, the casting material is poured into a mold, and is cured at high temperature, and the mold is removed to obtain the high compressive strength transparent organic material. Specifically, pouring the casting material into a flat plate-shaped mold, curing in stages according to the modes of heating at 80 ℃, keeping the temperature for 2h, heating at 115 ℃, keeping the temperature for 2h, heating at 160 ℃ and keeping the temperature for 26h, cooling and demolding to obtain the high-compression-strength transparent organic material.
The performance of the low temperature resistant transparent TPU film prepared by the method is tested, and the test data is as follows:
test items Results
Light transmittance% 92
Haze% of 0.1
Tensile strength Mpa 125
Elongation at break% 4.5
Compressive strength Mpa 201
Example 2
Weighing the following components in percentage by weight: 80% isocyanate (IPDI); 9% of 1, 5-pentanediol; 10% trimethylolpropane; 0.5% of antioxidant; 0.5% of an ultraviolet additive.
Please refer to fig. 1, which is a flowchart illustrating a method for preparing a high compressive strength transparent organic material according to an embodiment of the present application. The high compressive strength transparent organic material was prepared according to the above formulation, and the preparation method 1 of the high compressive strength transparent organic material includes the following steps S1 to S6. Wherein:
in step S1, the small-molecule chain extender is dehydrated in vacuum so that the mass fraction of water is 0.05% or less. Specifically, 1, 5-pentanediol is added into a three-neck flask provided with a stirrer and a thermometer, the mixture is heated to 110 ℃, dehydrated for 2 to 3 hours under vacuum, the mass fraction of water in the material is not higher than 0.05 percent, and cooled to 80 ℃ for standby.
In step S2, isocyanate and the dehydrated small molecule chain extender are uniformly mixed, heated and stirred to obtain a first material. Specifically, the 1, 5-pentanediol dehydrated in the step S1 is added into metered IPDI, the temperature is kept at 80 ℃, the mixture is heated and stirred for reaction for 2-3 hours, and after the theoretical NCO content is reached, the first material is obtained for standby.
In step S3, the crosslinking agent, the antioxidant, and the ultraviolet additive are mixed, heated, and stirred to obtain a second material. Specifically, trimethylolpropane, antioxidant 1010 and UV-328 are added into a beaker, and stirred at 80 ℃ until the materials are melted, so that a second material is obtained for later use.
In step S4, the second material and the first material are mixed, heated and stirred to obtain the castable. Specifically, the second material is added into a three-neck flask of the first material, the first material and the second material are stirred by a stirrer in the three-neck flask at 80 ℃ until the materials are clear, and then bubbles are removed in vacuum for 5 minutes to obtain the castable.
In step S5, the casting material is poured into a mold, and is cured at high temperature, and the mold is removed to obtain the high compressive strength transparent organic material. Specifically, pouring the casting material into a flat plate-shaped mold, curing in stages according to the modes of heating at 80 ℃, keeping the temperature for 2h, heating at 115 ℃, keeping the temperature for 2h, heating at 160 ℃ and keeping the temperature for 26h, cooling and demolding to obtain the high-compression-strength transparent organic material.
The performance of the low temperature resistant transparent TPU film prepared by the method is tested, and the test data is as follows:
test items Results
Light transmittance% 92
Haze%) 0.1
Tensile strength Mpa 120
Elongation at break% 6.5
Compressive strength Mpa 185
By combining the test results of the above example 1 and example 2, the high compressive strength transparent organic material prepared according to the formulation of the high compressive strength transparent organic material and the preparation method thereof has a light transmittance of more than 90%, a haze of about 0.1%, a tensile strength of not less than 120Mpa, an elongation at break of about 5%, and a compressive strength of more than 180 Mpa.
In summary, the present application provides a formulation for a high compressive strength transparent organic material and a method for preparing the same. Compared with the existing transparent organic material, the high-compression-strength transparent organic material prepared by the method can greatly improve the compression strength, so that the material is suitable for some special fields, and the vacancy of the high-compression-strength transparent organic material is filled. Meanwhile, the preparation method is simple and easy to operate.
It should be noted that, in this document, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other like elements in a process, method, article, or apparatus that comprises the element.
While the present embodiments have been described with reference to the accompanying drawings, it is to be understood that the invention is not limited to the precise embodiments described above, which are meant to be illustrative and not restrictive, and that various changes may be made therein by those skilled in the art without departing from the spirit and scope of the invention as defined by the appended claims.

Claims (10)

1. The formula of the transparent organic material with high compressive strength is characterized by comprising the following components in percentage by weight:
75-80% of isocyanate;
5-10% of micromolecular chain extender;
10-15% of a cross-linking agent;
0.5% of antioxidant;
0.5% of an ultraviolet additive.
2. The formulation for high compressive strength transparent organic material of claim 1, wherein the isocyanate comprises one or more of dicyclohexylmethane diisocyanate, p-phenylene diisocyanate, isophorone diisocyanate, 1, 5-naphthalene diisocyanate.
3. The formulation of a high compressive strength transparent organic material of claim 1, wherein the small molecule chain extender comprises one or more of ethylene glycol, propylene glycol, 1, 4-butanediol, diethylene glycol, 1, 3-butanediol, 1, 5-pentanediol, 2-dimethyl-1, 3-propanediol, methyl propanediol, or diethylene glycol (diethylene glycol).
4. The formulation of a high compressive strength transparent organic material of claim 1, wherein the cross-linking agent comprises one or more of glycerol, trimethylolethane, trimethylolpropane, MOCA, diisopropanolamine.
5. The formulation of a high compressive strength transparent organic material of claim 1, wherein said antioxidant is antioxidant 1010 and said ultraviolet additive is UV-328.
6. A preparation method of a transparent organic material with high compressive strength is characterized by comprising the following steps:
(a) weighing the raw materials according to the formulation of the transparent organic material with high compressive strength as claimed in any one of the above claims 1 to 5;
(b) vacuum dehydrating the micromolecule chain extender to enable the mass fraction of water to be less than or equal to 0.05%;
(c) uniformly mixing the isocyanate and the dehydrated micromolecule chain extender, and heating and stirring to obtain a first material;
(d) mixing the cross-linking agent, the antioxidant and the ultraviolet additive, and heating and stirring to obtain a second material;
(e) mixing the second material with the first material, and heating and stirring to obtain a castable;
(f) and pouring the castable into a mold, curing at high temperature in stages, and removing the mold to obtain the high-compressive-strength transparent organic material.
7. The method as claimed in claim 6, wherein in the step (b), the small molecule chain extender is added into a three-neck flask equipped with a stirrer and a thermometer during vacuum dehydration, heated to 110 ℃ and dehydrated for 2-3h under vacuum, and cooled to 80 ℃ for standby.
8. The method for preparing a high compressive strength transparent organic material according to claim 6, wherein the heating stirring temperature in the steps (c) to (e) is 80 ℃.
9. The method according to claim 6, wherein in the step (e), the second material is further vacuum bubble-removed after the heating and stirring of the first material and the second material.
10. The method according to claim 6, wherein the step (f) is a step curing process in which the high-compressive-strength transparent organic material is heated at 80 ℃ for 2 hours, heated at 115 ℃ for 2 hours, heated at 160 ℃ for 26 hours, and cured at a high temperature.
CN202210785403.6A 2022-07-05 2022-07-05 Formula of high-compressive-strength transparent organic material and preparation method thereof Pending CN114957585A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102604038A (en) * 2012-03-01 2012-07-25 深圳市乐普泰科技股份有限公司 Transparent polyurethane elastomer and preparation method as well as application
CN112812266A (en) * 2021-01-05 2021-05-18 江苏铁锚玻璃股份有限公司 IPDI type transparent high-strength polyurethane plate and preparation method thereof
CN113563554A (en) * 2021-07-15 2021-10-29 盛鼎高新材料有限公司 Preparation method of interlayer optical material of safety glass
CN114634611A (en) * 2022-04-20 2022-06-17 江苏铁锚玻璃股份有限公司 Formula and preparation method of oriented stretch polyurethane plate

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102604038A (en) * 2012-03-01 2012-07-25 深圳市乐普泰科技股份有限公司 Transparent polyurethane elastomer and preparation method as well as application
CN112812266A (en) * 2021-01-05 2021-05-18 江苏铁锚玻璃股份有限公司 IPDI type transparent high-strength polyurethane plate and preparation method thereof
CN113563554A (en) * 2021-07-15 2021-10-29 盛鼎高新材料有限公司 Preparation method of interlayer optical material of safety glass
CN114634611A (en) * 2022-04-20 2022-06-17 江苏铁锚玻璃股份有限公司 Formula and preparation method of oriented stretch polyurethane plate

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Application publication date: 20220830