CN105646837B - A kind of preparation method of ultra-thin polyurethane material - Google Patents
A kind of preparation method of ultra-thin polyurethane material Download PDFInfo
- Publication number
- CN105646837B CN105646837B CN201610100551.4A CN201610100551A CN105646837B CN 105646837 B CN105646837 B CN 105646837B CN 201610100551 A CN201610100551 A CN 201610100551A CN 105646837 B CN105646837 B CN 105646837B
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- China
- Prior art keywords
- polyether polyol
- ultra
- polyurethane material
- preparation
- isocyanates
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Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
- C08G18/76—Polyisocyanates or polyisothiocyanates cyclic aromatic
- C08G18/7657—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
- 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
- C08G18/4812—Mixtures of polyetherdiols with polyetherpolyols having at least three hydroxy groups
-
- 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
- C08G2110/00—Foam properties
- C08G2110/0083—Foam properties prepared using water as the sole blowing agent
Abstract
A kind of preparation method of ultra-thin polyurethane material, this method is first by polyether polyol, water, stabilizer, catalyst, chain extender by weight 70~90:1~5:0.7~2:0.01~0.05:10~20 carry out high-precision measuring mixing to obtain mixture under 40~70 DEG C, 15~30MPa, 10~40 parts of isocyanates high-speed stirreds are added into mixture again to form reactant, again by reactant vacuum defoamation, ultra-thin polyurethane material then can be prepared using reaction equation precision coating technique.This method not only makes polyurethane material thinner thickness, has high compression ratio, shock resistance and sealing performance and resilience good, and ensure that isocyanates fully react, the distribution of cells that is formed it is uniform enough.
Description
Technical field
The invention belongs to ultra-thin materials preparation fields, and in particular to a kind of preparation method of ultra-thin polyurethane material.
Background technology
Mobile phone products are more and more thinner at present, and to anti-ballistic materials therein, the requirement of sealing material is also higher and higher, existing
The foam product of technology is generally thicker, and domestic ideal ultrathin products generally also can only achieve 1mm, can not meet current technology
Demand.
Chinese patent：Application publication number is CN104987702A, and data of publication of application is that the invention on October 21st, 2015 is special
Profit discloses a kind of polyurethane foam and preparation method thereof, which is polymerize by component A and component B forms, component A packets
Including the isocyanates containing two or more isocyanate groups, component B includes polyethylene and polyalcohol, when preparation,
It first is placed in container and stirs evenly component A and component B to form performed polymer, then foamed gas is filled with into the container, make
Pressure in the container reaches 1MPa~10MPa, is kept for 5 minutes~15 minutes, then by performed polymer by pipeline extremely
Coating machine, and performed polymer is coated on base material by the coating machine, finally it is coated with the base material of the performed polymer
It is placed in progress curing molding in curing oven.Although the invention is made by adding polyethylene in isocyanates and polyalcohol
The intensity for obtaining the microstructure for the polyurethane foam that isocyanates and polymerization are formed improves, so as to improve polyurethane foam
Wearability, but still have the following defects：
Component A and component B is first directly mixed and forms performed polymer by this method, i.e. use disposably mixes raw material
Mode, it is uniform enough which so that isocyanates can not disperse in system, thus can not ensure isocyanates fully react,
The distribution of cells of formation is uniform enough.
Invention content
The purpose of the present invention is overcome the abscess point of the existing technology that can not ensure isocyanates and fully react, formed
The sufficiently uniform problem of cloth, provide it is a kind of can effectively ensure that isocyanates fully react, the distribution of cells that is formed it is sufficiently uniform
The preparation method of ultra-thin polyurethane material.
In order to achieve the above object, technical scheme is as follows：
A kind of preparation method of ultra-thin polyurethane material, includes the following steps successively：
Step 1: by polyether polyol, water, stabilizer, catalyst, chain extender by weight 70~90:1~5: 0.7
~2:0.01~0.05:10~20 carry out high-precision measuring mixing to obtain mixture under 40~70 DEG C, 15~30MPa；
It is taken off to form reactant, then by reactant vacuum Step 2: isocyanates high-speed stirred is first added into mixture
Then ultra-thin polyurethane material can be prepared using reaction equation precision coating technique in bubble, wherein the isocyanates adds
The weight part ratio for entering amount and polyether polyol in mixture is 10~40:70~90.
In the step 1, incorporation time is 10~30min；
In the step 2, speed of agitator is more than or equal to 4000r/min, and mixing time is 1~5min.
The polyether polyol distinguishes precentagewise content by polyether polyol A, polyether polyol B, polyether polyol C
45%~65%, 10%~50%, 5%~25% mixes, wherein polyether polyol A is trifunctional of the hydroxyl value 250~350
Polyether polyol, polyether polyol B are trifunctional polyether polyol of the hydroxyl value 25~80, and polyether polyol C is that hydroxyl value exists
25~80 two functional group's polyether polyol.
The polyether polyol A is SK Y-1030 polyether polyol, and the polyether polyol B is POP3628 polyether polyols
Alcohol, the polyether polyol C are polypropylene glycol PPG3000 polyether polyol.
The isocyanates is methyl diphenylene diisocyanate, and the stabilizer is dimethyl polysiloxane and polyethers
Block copolymer, the catalyst are triethylenediamine, dibutyl tin laurate or stannous octoate, and the water is handed over for ion
Change water or distilled water.
Compared with prior art, beneficial effects of the present invention are：
Raw material in addition to isocyanates is first carried out high-precision by a kind of preparation method of ultra-thin polyurethane material of the present invention
Metering mixing, adds isocyanates mixing, uses reaction equation precision coating technique that can be prepared after vacuum defoamation ultra-thin
Polyurethane material, on the one hand, this method not only makes the initial viscosity of whole system very low by the adjustment of formula, is prepared
Polyurethane material uncompressed state thickness up to 0.1mm hereinafter, and making polyurethane material inner cell in half-open
Pore structure has high compression ratio, shock resistance and favorable sealing property, while can also keep excellent resilience, another party
Face, this method ensure that isocyanates can disperse enough uniformly in system in such a way that substep mixes so that formation
Distribution of cells is uniform enough, so that it is guaranteed that polyurethane material has excellent mechanical performance.Therefore, the present invention not only makes poly- ammonia
Ester material thinner thickness has high compression ratio, shock resistance and sealing performance and resilience good, and ensure that isocyanide
The distribution of cells that acid esters fully reacts, is formed is uniform enough.
Specific implementation mode
The present invention will be further described in detail with reference to the specific embodiments.
A kind of preparation method of ultra-thin polyurethane material, includes the following steps successively：
Step 1: by polyether polyol, water, stabilizer, catalyst, chain extender by weight 70~90:1~5:0.7
~2:0.01~0.05:10~20 carry out high-precision measuring mixing to obtain mixture under 40~70 DEG C, 15~30MPa；
It is taken off to form reactant, then by reactant vacuum Step 2: isocyanates high-speed stirred is first added into mixture
Then ultra-thin polyurethane material can be prepared using reaction equation precision coating technique in bubble, wherein the isocyanates adds
The weight part ratio for entering amount and polyether polyol in mixture is 10~40:70~90.
In the step 1, incorporation time is 10~30min；
In the step 2, speed of agitator is more than or equal to 4000r/min, and mixing time is 1~5min.
The polyether polyol distinguishes precentagewise content by polyether polyol A, polyether polyol B, polyether polyol C
45%~65%, 10%~50%, 5%~25% mixes, wherein polyether polyol A is trifunctional of the hydroxyl value 250~350
Polyether polyol, polyether polyol B are trifunctional polyether polyol of the hydroxyl value 25~80, and polyether polyol C is that hydroxyl value exists
25~80 two functional group's polyether polyol.
The polyether polyol A is SK Y-1030 polyether polyol, and the polyether polyol B is POP3628 polyether polyols
Alcohol, the polyether polyol C are polypropylene glycol PPG3000 polyether polyol.
The isocyanates is methyl diphenylene diisocyanate, and the stabilizer is dimethyl polysiloxane and polyethers
Block copolymer, the catalyst are triethylenediamine, dibutyl tin laurate or stannous octoate, and the water is handed over for ion
Change water or distilled water.
The principle of the present invention is described as follows：
The present invention provides a kind of methods preparing ultra-thin polyurethane material by one-step method, and obtained product is uncompressed
Up to 0.1mm hereinafter, product abscess aperture is only 70~120um, and distribution uniform has high compression for thickness under state
Than shock resistance, sealing performance and resilience are good.Each step is described as follows：
Step 1：
To accurately control isocyanate index（The equivalents of equivalents/polyalcohol of isocyanate index=isocyanates）,
It is accurately controlled the viscosity of reaction system simultaneously, it is ensured that the efficiency entirely reacted, the step is by other in addition to isocyanates
Raw material carries out high-precision measuring mixing.
Step 2：
In the step, it is enough uniform that rear addition isocyanates can be such that it is mixed in system, and fully reacts, and obtains more
Good dispersibility, this is to lead to the sufficiently uniform key factor of distribution of cells.
It is also beneficial to ensure that distribution of cells is uniform in 4000r/min or more in addition, controlling speed of agitator.
Embodiment 1：
A kind of preparation method of ultra-thin polyurethane material, follows the steps below successively：
Step 1: by polyether polyol, water, stabilizer, catalyst, chain extender by weight 70:1:0.7:0.01:
10 carry out high-precision measuring mixing 20min to obtain mixture under 60 DEG C, 20MPa, wherein the stabilizer is silicone oil, institute
It is triethylenediamine to state catalyst, and the water is ion exchange water；
Step 2: isocyanates is first added into mixture stirs 5min to form reactant with the rotating speed of 4000r/min,
Again by reactant vacuum defoamation, ultra-thin polyurethane material then can be prepared using reaction equation precision coating technique, wherein
The polyether polyol by polyether polyol A, polyether polyol B, polyether polyol C difference precentagewise content 45%, 30%,
25% mixes, wherein polyether polyol A is SK Y-1030 polyether polyol（Hydroxyl value 290~330）, polyether polyol B is
（Hydroxyl value 25~29）POP3628 polyether polyol, polyether polyol C are（Hydroxyl value 54~58）Polypropylene glycol PPG3000 polyethers is more
First alcohol, the isocyanates are methyl diphenylene diisocyanate, and polyethers is more in the addition and mixture of the isocyanates
The weight part ratio of first alcohol is 10:70.
Embodiment 2：
Step with embodiment 1, the difference is that：
In the step 1, polyether polyol, water, stabilizer, catalyst, chain extender weight part ratio be 90:5: 2:
0.05:20, mixing temperature is 70 DEG C, pressure 30MPa, incorporation time 10min, and catalyst is dibutyl tin laurate；
In the step 2, speed of agitator 5000r/min, mixing time 1min, polyether polyol A, polyether polyols
Alcohol B, polyether polyol C degree be respectively 65%, 10%, 25%, polyethers is more in the addition and mixture of isocyanates
The weight part ratio of first alcohol is 40:90.
Embodiment 3：
Step with embodiment 1, the difference is that：
In the step 1, polyether polyol, water, stabilizer, catalyst, chain extender weight part ratio be 80:3: 1.5:
0.03:15, mixing temperature is 40 DEG C, pressure 15MPa, incorporation time 30min, and catalyst is stannous octoate, and water is distillation
Water；
In the step 2, mixing time 5min, polyether polyol A, polyether polyol B, polyether polyol C percentage
It is respectively 45%, 50%, 5% than content, the weight part ratio of polyether polyol is 25 in the addition and mixture of isocyanates:80.
To carrying out compressing force deflection test using ultra-thin polyurethane products made from above-described embodiment method, the results showed that：
The product is compressed to pressure suffered when 10% thickness and is not more than 0.1N/mm2, the compression set at 25 DEG C is not more than
3%（50% is compressed at 25 DEG C, is kept for 22 hours）, meanwhile, which can keep at least 90% original depth (to be compressed at 70 DEG C
50%, kept for 22 hours).
Claims (3)
1. a kind of preparation method of ultra-thin polyurethane material, it is characterised in that：
The preparation method includes the following steps successively：
Step 1: by polyether polyol, water, stabilizer, catalyst, chain extender by weight 70~90:1~5:0.7~2:
0.01~0.05:10~20 carry out high-precision measuring mixing to obtain mixture under 40~70 DEG C, 15~30MPa, wherein institute
Polyether polyol is stated by SK Y-1030 polyether polyol, POP3628 polyether polyol, polypropylene glycol PPG3000 polyether polyol
Precentagewise content 45%~65%, 10%~50%, 5%~25% mixes respectively；
Step 2: isocyanates high-speed stirred is first added into mixture to form reactant, then by reactant vacuum defoamation, with
Use reaction equation precision coating technique that ultra-thin polyurethane material can be prepared afterwards, wherein the addition of the isocyanates
Weight part ratio with polyether polyol in mixture is 10~40:70~90.
2. a kind of preparation method of ultra-thin polyurethane material according to claim 1, it is characterised in that：
In the step 1, the incorporation time for obtaining mixture is 10~30min；
In the step 2, speed of agitator is more than or equal to 4000r/min, and mixing time is 1~5min.
3. a kind of preparation method of ultra-thin polyurethane material according to claim 1 or 2, it is characterised in that：The isocyanide
Acid esters is methyl diphenylene diisocyanate, and the stabilizer is the block copolymer of dimethyl polysiloxane and polyethers, described
Catalyst is triethylenediamine, dibutyl tin laurate or stannous octoate, and the water is ion exchange water or distilled water.
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| CN201610100551.4A CN105646837B (en) | 2016-02-24 | 2016-02-24 | A kind of preparation method of ultra-thin polyurethane material |
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| CN201610100551.4A CN105646837B (en) | 2016-02-24 | 2016-02-24 | A kind of preparation method of ultra-thin polyurethane material |
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| CN105646837B true CN105646837B (en) | 2018-08-17 |
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| CN112225869B (en) * | 2020-10-14 | 2022-04-12 | 广德祥源新材科技有限公司 | Polyurethane microporous foam with uniform pore diameter and preparation method thereof |
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| JPH078554B2 (en) * | 1986-01-29 | 1995-02-01 | 東洋化学株式会社 | Ultra-thin pressure-sensitive adhesive tape for skin attachment |
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| CN104512076B (en) * | 2013-09-26 | 2018-05-22 | 美国圣戈班性能塑料公司 | Ultrathin foam gasket and adhesive tape |
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| US5231159A (en) * | 1990-12-27 | 1993-07-27 | The Gates Rubber Company | High temperature resistant molded elastomer |
| CN101250253A (en) * | 2008-04-01 | 2008-08-27 | 江苏德翔聚氨酯塑胶有限公司 | Formula of cold curing foam and forming technique |
| CN101914282A (en) * | 2010-08-18 | 2010-12-15 | 漳州华德高分子应用材料科技有限公司 | Natural plant oil based hydrophile low-resilience foam and preparation method thereof |
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