CN108641062A - A kind of middle modulus, the preparation method of high springback wet method resin - Google Patents
A kind of middle modulus, the preparation method of high springback wet method resin Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
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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
- C08G18/08—Processes
- C08G18/10—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step
- C08G18/12—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step using two or more compounds having active hydrogen in the first polymerisation step
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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
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Abstract
A kind of middle modulus, the preparation method of high springback wet method resin are specifically comprising raw material：Polyester polyol A, polyester polyol B, methyl diphenylene diisocyanate A, N, N dimethylformamides, 1,4 butanediols, antioxidant, methyl diphenylene diisocyanate B；The wet method resin has physical property good；Abscess fine uniform, embossing performance are good, elasticity is good, high resilience, setting rate, take off the good advantage of DMF speed.Wet method tree tool is soft, embossing performance is good, elasticity is good, particularly suitable ground luggage, shoes leather；The transparent colloidal state of this wet method resin, solid content 30+1%, viscosity is 16 22 ten thousand cps/25 DEG C, modulus is 40 50kg/cm2, 450 ㎏ of fracture strength ＞/cm2, extension at break ＞ 400, this wet method resin has physical property good, the feature that feel is thick and solid, embossing performance is good, applied widely.
Description
Technical field
The present invention relates to a kind of development fields of resin, more particularly to a kind of middle modulus, the synthesis side of high rebound resin
Method.
Background technology
It is higher and higher with the requirement of polyurethane wet resin for leather with the development of pu synthetic leather industries, it is original wet
Method resin, if improve resin at flesh, it is such it will cause forming a large amount of larger-size abscesses inside synthetic leather
Synthetic leather has the shortcomings that resilience is poor, peel strength is low, cortex hardening.
Therefore, in view of the shortcomings of the prior art, a kind of middle modulus of offer, the preparation method of high springback wet method resin are existing to overcome
There is technical deficiency very necessary.
Invention content
A kind of middle modulus, high springback wet method tree are provided it is an object of the invention to avoid shortcoming in the prior art
The preparation method of fat, the wet method resin have abscess fine and closely woven, and resilience is good, the fast feature of setting rate.
The above-mentioned purpose of the present invention is realized by following technological means.
A kind of middle modulus, the preparation method of high springback wet method resin, the prepared transparent colloidal of wet method resin are provided
State, solid content 30+1%, viscosity is cps/25 DEG C of 16-22 ten thousand, modulus is 40-50kg/c ㎡, 450 ㎏ of fracture strength ＞/c
㎡, extension at break ＞ 400, step, which is specifically made, is：
Polyester polyol A and polyester polyol B are heated to temperature T1 by first step in sealing reaction unit, are stirred
And to material dissolution；
Second step, is added methyl diphenylene diisocyanate A in seal reaction unit, and from sealing reaction unit
Bottom is passed through nitrogen from bottom to top, and the air-flow of nitrogen is 30-80m3/ min, and stirring simultaneously is warming up to T2,60-90 points of heat preservation
Clock；
The mixing of n,N-Dimethylformamide, 1,4-butanediol, antioxidant is added in third step in sealing reaction unit
Object is heated to T3, fully dissolves and stir evenly；
The inner air in sealing reaction unit is extracted, the air pressure in sealing reaction unit is made to be maintained at -30 to -50Pa,
And continue 30-35 minutes；
Methyl diphenylene diisocyanate B is added into sealing reaction unit for four steps, and stirring is warming up to temperature T4,
Then 60-90 minutes are kept the temperature；
Whether the 5th step, sample detection, the viscosity for detecting sample reach cps/25 DEG C of 20-25 ten thousand；
When viscosity reaches ten thousand cps/25 DEG C of 20-25, methanol is added, is cooled to temperature T5, auxiliary agent is added, stirs 30 points
Clock stirs evenly, and obtains wet method resin.
Preferably, in above-mentioned first step be specially in sealing reaction unit by the polyester polyols of 7.5-12.5 mass parts
The polyester polyol B of alcohol A and 8.5-13.5 mass parts is heated to temperature T1, stirs and to material dissolution；
It is specially the diphenylmethane diisocyanate that 3.5-5.5 mass parts are added in sealing reaction unit in second step
Ester A, and it is passed through nitrogen from bottom to top from the bottom of sealing reaction unit, the air-flow of nitrogen is 30-80m3/ min, and stir simultaneously
It is warming up to T2, keeps the temperature 60-90 minutes；
In third step be specially in seal reaction unit addition 15-25 mass parts N,N-dimethylformamide,
The mixture of the 1,4-butanediol of 1.5-2.5 mass parts, the antioxidant of 0.1-0.4 mass parts, is heated to T3, fully dissolves and stir
It mixes uniformly；
The inner air in sealing reaction unit is extracted, the air pressure in sealing reaction unit is made to be maintained at -30 to -50Pa,
And continue 30-35 minutes；
It is specially the diphenylmethane diisocyanate that 2.4-3.4 mass parts are added into sealing reaction unit in four steps
Ester B, stirring are warming up to temperature T4, then keep the temperature 60-90 minutes；
Specifically, whether sample detection, the viscosity for detecting sample reach cps/25 DEG C of 20-25 ten thousand in 5th step；
When sample viscosity is not up to ten thousand cps/25 DEG C of 20-25, '-diphenylmethane diisocyanate D is added, with viscosity
When constantly rising to 500,000 cps/70 DEG C, organic solvent C is added in two portions, until viscosity reaches cps/25 DEG C of 20-25 ten thousand；
When viscosity reaches ten thousand cps/25 DEG C of 20-25, methanol is added, is cooled to temperature T5, auxiliary agent is added, stirs 30 points
Clock stirs evenly, and obtains modulus in finished product, high springback wet method resin.
It is another preferred, by the polyester polyol of 10 mass parts specially in sealing reaction unit in above-mentioned first step
The A and polyester polyol B of 11 mass parts is heated to temperature T1, stirs and to material dissolution；
It is specially the methyl diphenylene diisocyanate A that 4.4 mass parts are added in sealing reaction unit in second step,
And it is passed through nitrogen from bottom to top from the bottom of sealing reaction unit, the air-flow of nitrogen is 75m3/ min, and stirring is warming up to simultaneously
T2 keeps the temperature 60-90 minutes；
It is specially N,N-dimethylformamide, 1.8 matter that 20 mass parts are added in sealing reaction unit in third step
The mixture of the 1,4-butanediol of amount part, the antioxidant of 0.1 mass parts, is heated to T3, fully dissolves and stir evenly；
The inner air in sealing reaction unit is extracted, the air pressure in sealing reaction unit is made to be maintained at -30 to -50Pa,
And continue 30-35 minutes；
It is specially the methyl diphenylene diisocyanate B that 2.8 mass parts are added into sealing reaction unit in four steps,
Stirring is warming up to temperature T4, then keeps the temperature 60-90 minutes；
Specifically, whether sample detection, the viscosity for detecting sample reach cps/25 DEG C of 20-25 ten thousand in 5th step；
When sample viscosity is not up to ten thousand cps/25 DEG C of 20-25, '-diphenylmethane diisocyanate D is added, with viscosity
When constantly rising to 500,000 cps/70 DEG C, organic solvent C is added in two portions, until viscosity reaches cps/25 DEG C of 20-25 ten thousand；
When viscosity reaches ten thousand cps/25 DEG C of 20-25, methanol is added, is cooled to temperature T5, auxiliary agent is added, stirs 30 points
Clock stirs evenly, and obtains modulus in finished product, high springback wet method resin.
It is another preferred, the polyester that polyester polyol A is model SP-230 in above-mentioned steps one and molecular weight is 3000
Polyalcohol；
The polyester polyol that polyester polyol B is model SP-220 in step 1 and molecular weight is 2000；
Temperature T1 is 50-70 DEG C in step 1.
It is another preferred, OH in methyl diphenylene diisocyanate A in above-mentioned steps two:NCO ratios are 1:2 diphenylmethyl
Alkane diisocyanate；
T2 is 70-80 DEG C in step 2.
Antioxidant is 2,6 di tert butyl 4 methyl phenol in step 3；
T3 is 50-70 DEG C in step 3.
Methyl diphenylene diisocyanate B is pure methyl diphenylene diisocyanate in step 4；
T3 is 70-80 DEG C in step 4.
'-diphenylmethane diisocyanate D is OH in step 5：NCO ratios are 1：0.98 methyl diphenylene diisocyanate；
Organic solvent C is N,N-dimethylformamide in step 5；
T5≤50 DEG C in step 5；
Auxiliary agent is the model PY-1002 of content 65% in step 5.
The present invention a kind of middle modulus, the preparation method of high springback wet method resin, be comprising raw material specifically：Polyester polyol
A, polyester polyol B, methyl diphenylene diisocyanate A, N,N-dimethylformamide, 1,4- butanediols, antioxidant, diphenyl
Methane diisocyanate B；The wet method resin has physical property good；Abscess fine uniform, embossing performance be good, the good, high resilience of elasticity,
The good advantage of setting rate, de- DMF speed.Wet method tree tool is soft, embossing performance is good, elastic good, particularly suitable ground case
Packet, shoes leather.
Specific implementation mode
The invention will be further described with the following Examples.
Embodiment 1.
A kind of middle modulus, the preparation method of high springback wet method resin, the prepared transparent colloidal state of wet method resin, Gu
Content is 30+1%, and viscosity is cps/25 DEG C of 16-22 ten thousand, modulus is 40-50kg/c ㎡, 450 ㎏ of fracture strength ＞/c ㎡, is broken
＞ 400 is extended, specifically obtained step is：
Polyester polyol A and polyester polyol B are heated to temperature T1 by first step in sealing reaction unit, are stirred
And to material dissolution；
Second step, is added methyl diphenylene diisocyanate A in seal reaction unit, and from sealing reaction unit
Bottom is passed through nitrogen from bottom to top, and the air-flow of nitrogen is 30-80m3/min, and stirring simultaneously is warming up to T2,60-90 points of heat preservation
Clock；It is passed through nitrogen by the bottom of autoreaction device while methyl diphenylene diisocyanate A is added, enables to seal
Material reaction in reaction unit is uniformly abundant, and to keep lasting hyperbar state inside reaction unit so that anti-
It answers the global density of the material inside device to increase, forms internal compression, ensured that the abscess of the finished product of wet method resin is fine and closely woven.
The mixing of n,N-Dimethylformamide, 1,4-butanediol, antioxidant is added in third step in sealing reaction unit
Object is heated to T3, fully dissolves and stir evenly；
The inner air in sealing reaction unit is extracted, the air pressure in sealing reaction unit is made to be maintained at -30 to -50Pa,
And continue 30-35 minutes.
In internal hyperbaric environment, the material in reaction unit is kept fully to react, in subsequent abstraction reaction device
Inner air keeps air pressure inside -30 to -50Pa, and continues 30-35 minutes, by the air pressure inside environment of moment, improves
The resilience performance of finished product wet method resin.
Methyl diphenylene diisocyanate B is added into sealing reaction unit for four steps, and stirring is warming up to temperature T4,
Then 60-90 minutes are kept the temperature；
Whether the 5th step, sample detection, the viscosity for detecting sample reach cps/25 DEG C of 20-25 ten thousand；
When viscosity reaches ten thousand cps/25 DEG C of 20-25, methanol is added, is cooled to temperature T5, auxiliary agent is added, stirs 30 points
Clock stirs evenly, and obtains wet method resin.
Specifically, by the polyester polyols of 7.5-12.5 mass parts specially in sealing reaction unit in above-mentioned first step
The polyester polyol B of alcohol A and 8.5-13.5 mass parts is heated to temperature T1, stirs and to material dissolution；
It is specially the diphenylmethane diisocyanate that 3.5-5.5 mass parts are added in sealing reaction unit in second step
Ester A, and it is passed through nitrogen from bottom to top from the bottom of sealing reaction unit, the air-flow of nitrogen is 30-80m3/ min, and stir simultaneously
It is warming up to T2, keeps the temperature 60-90 minutes；
In third step be specially in seal reaction unit addition 15-25 mass parts N,N-dimethylformamide,
The mixture of the 1,4-butanediol of 1.5-2.5 mass parts, the antioxidant of 0.1-0.4 mass parts, is heated to T3, fully dissolves and stir
It mixes uniformly；
The inner air in sealing reaction unit is extracted, the air pressure in sealing reaction unit is made to be maintained at -30 to -50Pa,
And continue 30-35 minutes；
It is specially the diphenylmethane diisocyanate that 2.4-3.4 mass parts are added into sealing reaction unit in four steps
Ester B, stirring are warming up to temperature T4, then keep the temperature 60-90 minutes；
Specifically, whether sample detection, the viscosity for detecting sample reach cps/25 DEG C of 20-25 ten thousand in 5th step；
When sample viscosity is not up to ten thousand cps/25 DEG C of 20-25, '-diphenylmethane diisocyanate D is added, with viscosity
When constantly rising to 500,000 cps/70 DEG C, organic solvent C is added in two portions, until viscosity reaches cps/25 DEG C of 20-25 ten thousand；
When viscosity reaches ten thousand cps/25 DEG C of 20-25, methanol is added, is cooled to temperature T5, auxiliary agent is added, stirs 30 points
Clock stirs evenly, and obtains modulus in finished product, high springback wet method resin.
The transparent colloidal state of this wet method resin, solid content 30+1%, viscosity is cps/25 DEG C of 16-22 ten thousand, modulus is
40-50kg/c ㎡, 450 ㎏ of fracture strength ＞/c ㎡, extension at break ＞ 400, by the way that nitrogen is added and keeps in preparation process
In the state of hyperbar so that the resin abscess finally prepared is fine and closely woven, and resilience is good.Made from this wet method process for preparing resins
Wet method resin has physical property good, the feature that feel is thick and solid, embossing performance is good, applied widely.
Embodiment 2.
A kind of middle modulus, the preparation method of high springback wet method resin, it is same as Example 1 to be specifically made step, different
Place is：It is specially in sealing reaction unit in first step by the polyester polyol A of 10 mass parts and 11 mass parts
Polyester polyol B is heated to temperature T1, stirs and to material dissolution；
It is specially the methyl diphenylene diisocyanate A that 4.4 mass parts are added in sealing reaction unit in second step,
And it is passed through nitrogen from bottom to top from the bottom of sealing reaction unit, the air-flow of nitrogen is 75m3/ min, and stirring is warming up to simultaneously
T2 keeps the temperature 60-90 minutes；
It is specially N,N-dimethylformamide, 1.8 matter that 20 mass parts are added in sealing reaction unit in third step
The mixture of the 1,4-butanediol of amount part, the antioxidant of 0.1 mass parts, is heated to T3, fully dissolves and stir evenly；
The inner air in sealing reaction unit is extracted, the air pressure in sealing reaction unit is made to be maintained at -30 to -50Pa,
And continue 30-35 minutes；
It is specially the methyl diphenylene diisocyanate B that 2.8 mass parts are added into sealing reaction unit in four steps,
Stirring is warming up to temperature T4, then keeps the temperature 60-90 minutes；
Specifically, whether sample detection, the viscosity for detecting sample reach cps/25 DEG C of 20-25 ten thousand in 5th step；
When sample viscosity is not up to ten thousand cps/25 DEG C of 20-25, '-diphenylmethane diisocyanate D is added, with viscosity
When constantly rising to 500,000 cps/70 DEG C, organic solvent C is added in two portions, until viscosity reaches cps/25 DEG C of 20-25 ten thousand；
When viscosity reaches ten thousand cps/25 DEG C of 20-25, methanol is added, is cooled to temperature T5, auxiliary agent is added, stirs 30 points
Clock stirs evenly, and obtains modulus in finished product, high springback wet method resin.
Polyester polyol A is kind hundred million polyester polyols that company's production model is SP-230 and molecular weight is 3000 in step 1
Alcohol；
Polyester polyol B is kind hundred million polyester polyols that company's production model is SP-220 and molecular weight is 2000 in step 1
Alcohol；
Temperature T1 is 50-70 DEG C in step 1.
It is another preferred, OH in methyl diphenylene diisocyanate A in above-mentioned steps two:NCO ratios are 1:2 diphenylmethyl
Alkane diisocyanate；
T2 is 70-80 DEG C in step 2.
Antioxidant is 2,6 di tert butyl 4 methyl phenol in step 3；
T3 is 50-70 DEG C in step 3.
Methyl diphenylene diisocyanate B is pure methyl diphenylene diisocyanate in step 4；
T3 is 70-80 DEG C in step 4.
'-diphenylmethane diisocyanate D is OH in step 5：NCO ratios are 1：0.98 methyl diphenylene diisocyanate；
Organic solvent C is N,N-dimethylformamide in step 5；
T5≤50 DEG C in step 5；
Auxiliary agent is the model PY-1002 of content 65% in step 5.
PY-1002 is the mixture of the polyoxyethylene oxypropylene ether of 1-6 mass parts and the toluene of 5-8 mass parts.
Methyl diphenylene diisocyanate produces for Wan Hua companies；1,4-butanediol produces for Meizhou Wan company.
The product of the present embodiment refers to art index：
Feature and advantage
1, high springback wet method resin, physical property is good；
2, feel is thick and solid, embossing performance is good, elasticity is good.
3, it is suitable for luggage, shoes are removed from office.
Resilience, setting rate, de- DMF speed of this product in processing performance, all reach good effect.
Finally it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention rather than is protected to the present invention
The limitation of range, although being explained in detail to the present invention with reference to preferred embodiment, those skilled in the art should manage
Solution, technical scheme of the present invention can be modified or replaced equivalently, without departing from technical solution of the present invention essence and
Range.
Claims (8)
1. a kind of middle modulus, the preparation method of high springback wet method resin, it is characterised in that：The prepared transparent glue of wet method resin
Body state, solid content 30+1%, viscosity is cps/25 DEG C of 16-22 ten thousand, modulus is 40-50kg/c ㎡, fracture strength ＞ 450
㎏/c ㎡, extension at break ＞ 400, step, which is specifically made, is：
Polyester polyol A and polyester polyol B are heated to temperature T1 by first step in sealing reaction unit, are stirred and extremely
Material dissolution；
Second step, in sealing reaction unit be added methyl diphenylene diisocyanate A, and from sealing reaction unit bottom
It is passed through nitrogen from bottom to top, the air-flow of nitrogen is 30-80m3/ min, and stirring is warming up to T2 simultaneously, keeps the temperature 60-90 minutes；
The mixture of n,N-Dimethylformamide, 1,4-butanediol, antioxidant is added in third step in sealing reaction unit,
It is heated to T3, fully dissolves and stirs evenly；
The inner air in sealing reaction unit is extracted, so that the air pressure in sealing reaction unit is maintained at -30 to -50Pa, and hold
It is 30-35 minutes continuous；
Methyl diphenylene diisocyanate B is added into sealing reaction unit for four steps, and stirring is warming up to temperature T4, then
Heat preservation 60-90 minutes；
Whether the 5th step, sample detection, the viscosity for detecting sample reach cps/25 DEG C of 20-25 ten thousand；
When viscosity reaches ten thousand cps/25 DEG C of 20-25, methanol is added, is cooled to temperature T5, auxiliary agent is added, stirs 30 minutes, stirs
It mixes uniformly, obtains wet method resin.
2. a kind of middle modulus according to claim 1, the preparation method of high springback wet method resin it is characterized in that：
By the polyester polyol A and 8.5- of 7.5-12.5 mass parts specially in sealing reaction unit in the first step
The polyester polyol B of 13.5 mass parts is heated to temperature T1, stirs and to material dissolution；
It is specially the diphenylmethane diisocyanate that 3.5-5.5 mass parts are added in sealing reaction unit in the second step
Ester A, and it is passed through nitrogen from bottom to top from the bottom of sealing reaction unit, the air-flow of nitrogen is 30-80m3/ min, and stir simultaneously
It is warming up to T2, keeps the temperature 60-90 minutes；
In the third step be specially in seal reaction unit addition 15-25 mass parts N,N-dimethylformamide,
The mixture of the 1,4-butanediol of 1.5-2.5 mass parts, the antioxidant of 0.1-0.4 mass parts, is heated to T3, fully dissolves and stir
It mixes uniformly；
The inner air in sealing reaction unit is extracted, so that the air pressure in sealing reaction unit is maintained at -30 to -50Pa, and hold
It is 30-35 minutes continuous；
It is specially the diphenylmethane diisocyanate that 2.4-3.4 mass parts are added into sealing reaction unit in the four steps
Ester B, stirring are warming up to temperature T4, then keep the temperature 60-90 minutes；
Specifically, whether sample detection, the viscosity for detecting sample reach cps/25 DEG C of 20-25 ten thousand in 5th step；
When sample viscosity is not up to ten thousand cps/25 DEG C of 20-25, '-diphenylmethane diisocyanate D is added, it is continuous with viscosity
When rising to 500,000 cps/70 DEG C, organic solvent C is added in two portions, until viscosity reaches cps/25 DEG C of 20-25 ten thousand；
When viscosity reaches ten thousand cps/25 DEG C of 20-25, methanol is added, is cooled to temperature T5, auxiliary agent is added, stirs 30 minutes, stirs
It mixes uniformly, obtains modulus in finished product, high springback wet method resin.
3. a kind of middle modulus according to claim 2, the preparation method of high springback wet method resin it is characterized in that：
Be specially in the first step in seal reaction unit gathering the polyester polyol A of 10 mass parts and 11 mass parts
Ester polyol B is heated to temperature T1, stirs and to material dissolution；
It is specially the methyl diphenylene diisocyanate A that 4.4 mass parts are added in sealing reaction unit in the second step,
And it is passed through nitrogen from bottom to top from the bottom of sealing reaction unit, the air-flow of nitrogen is 75m3/ min, and stirring is warming up to simultaneously
T2 keeps the temperature 60-90 minutes；
It is specially N,N-dimethylformamide, 1.8 matter that 20 mass parts are added in sealing reaction unit in the third step
The mixture of the 1,4-butanediol of amount part, the antioxidant of 0.1 mass parts, is heated to T3, fully dissolves and stir evenly；
The inner air in sealing reaction unit is extracted, so that the air pressure in sealing reaction unit is maintained at -30 to -50Pa, and hold
It is 30-35 minutes continuous；
It is specially the methyl diphenylene diisocyanate B that 2.8 mass parts are added into sealing reaction unit in the four steps,
Stirring is warming up to temperature T4, then keeps the temperature 60-90 minutes；
Specifically, whether sample detection, the viscosity for detecting sample reach cps/25 DEG C of 20-25 ten thousand in 5th step；
When sample viscosity is not up to ten thousand cps/25 DEG C of 20-25, '-diphenylmethane diisocyanate D is added, it is continuous with viscosity
When rising to 500,000 cps/70 DEG C, organic solvent C is added in two portions, until viscosity reaches cps/25 DEG C of 20-25 ten thousand；
When viscosity reaches ten thousand cps/25 DEG C of 20-25, methanol is added, is cooled to temperature T5, auxiliary agent is added, stirs 30 minutes, stirs
It mixes uniformly, obtains modulus in finished product, high springback wet method resin.
4. a kind of middle modulus according to claim 3, the preparation method of high springback wet method resin it is characterized in that：
The polyester polyol that polyester polyol A is model SP-230 in the step 1 and molecular weight is 3000；
The polyester polyol that polyester polyol B is model SP-220 in the step 1 and molecular weight is 2000；
Temperature T1 is 50-70 DEG C in the step 1.
5. a kind of middle modulus according to claim 4, the preparation method of high springback wet method resin it is characterized in that：
OH in methyl diphenylene diisocyanate A in the step 2:NCO ratios are 1:2 methyl diphenylene diisocyanate；
T2 is 70-80 DEG C in the step 2.
6. a kind of middle modulus according to claim 5, the preparation method of high springback wet method resin it is characterized in that：
Antioxidant is 2,6 di tert butyl 4 methyl phenol in the step 3；
T3 is 50-70 DEG C in the step 3.
7. a kind of middle modulus according to claim 6, the preparation method of high springback wet method resin it is characterized in that：
Methyl diphenylene diisocyanate B is pure methyl diphenylene diisocyanate in the step 4；
T3 is 70-80 DEG C in the step 4.
8. a kind of middle modulus according to claim 7, the preparation method of high springback wet method resin it is characterized in that：
'-diphenylmethane diisocyanate D is OH in the step 5：NCO ratios are 1：0.98 methyl diphenylene diisocyanate；
Organic solvent C is N,N-dimethylformamide in the step 5；
T5≤50 DEG C in the step 5；
Auxiliary agent is the model PY-1002 of content 65% in the step 5.
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| CN201810533266.0A Pending CN108641062A (en) | 2018-05-25 | 2018-05-25 | A kind of middle modulus, the preparation method of high springback wet method resin |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109853254A (en) * | 2019-02-28 | 2019-06-07 | 扬州工业职业技术学院 | A kind of middle hard mirror surface polyurethane wet bass and preparation method thereof |
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| CN102993398A (en) * | 2012-10-16 | 2013-03-27 | 福建国邦树脂有限公司 | Wet type polyurethane resin, production process and application method thereof |
| CN104844780A (en) * | 2015-05-22 | 2015-08-19 | 佛山市高明恒祥化工树脂有限公司 | Environment-friendly low-temperature wet stamping-discoloring polyurethane resin and preparation method for same |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102993398A (en) * | 2012-10-16 | 2013-03-27 | 福建国邦树脂有限公司 | Wet type polyurethane resin, production process and application method thereof |
| CN104844780A (en) * | 2015-05-22 | 2015-08-19 | 佛山市高明恒祥化工树脂有限公司 | Environment-friendly low-temperature wet stamping-discoloring polyurethane resin and preparation method for same |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109853254A (en) * | 2019-02-28 | 2019-06-07 | 扬州工业职业技术学院 | A kind of middle hard mirror surface polyurethane wet bass and preparation method thereof |
| CN109853254B (en) * | 2019-02-28 | 2021-08-03 | 扬州工业职业技术学院 | Medium-hard mirror polyurethane wet base and preparation method thereof |
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