CN106866916A - Easily extract the preparation method of the polyurethane resin for superfine fiber synthetic leather of marine facies - Google Patents

Easily extract the preparation method of the polyurethane resin for superfine fiber synthetic leather of marine facies Download PDF

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Publication number
CN106866916A
CN106866916A CN201710191593.8A CN201710191593A CN106866916A CN 106866916 A CN106866916 A CN 106866916A CN 201710191593 A CN201710191593 A CN 201710191593A CN 106866916 A CN106866916 A CN 106866916A
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China
Prior art keywords
polyurethane resin
superfine fiber
preparation
synthetic leather
marine facies
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CN201710191593.8A
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Inventor
沈连根
纪尚超
徐欣欣
石磊
李寿伟
周泉
张雪刚
武锦峰
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JIAXING HEXIN CHEMICAL INDUSTRY CO LTD
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JIAXING HEXIN CHEMICAL INDUSTRY CO LTD
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Priority to CN201710191593.8A priority Critical patent/CN106866916A/en
Publication of CN106866916A publication Critical patent/CN106866916A/en
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Abstract

A kind of preparation method of the easy polyurethane resin for superfine fiber synthetic leather for extracting marine facies, poly-dihydric alcohol, chain extender and diisocyanate, antioxidant, catalyst are heated in a solvent and is reacted, after being reacted to corresponding viscosity, use terminator terminating reaction, add other auxiliary agents, stir, obtain final products, wherein being additionally added be in mass raw material total amount 0.1%~10% water-soluble high-molecular material while other auxiliary agents are added after terminating reaction.Superfine fiber chemical leather is manufactured with polyurethane resin obtained in the method, water-soluble high-molecular material and polyurethane resin are coated on superfine fibre surface together during impregnation, in subsequent hot water water-washing process, water-soluble high-molecular material and DMF are taken away by the water together, tiny micropore is left in polyurethane surface, so that toluene is more easily accessible to superfine fiber fabric in extraction process, the polyolefin of dissolving is easier to be extracted, and greatly shortens the time that toluene extracts polyolefin.

Description

Easily extract the preparation method of the polyurethane resin for superfine fiber synthetic leather of marine facies
Technical field
The present invention relates to a kind of preparation method of the easy polyurethane resin for superfine fiber synthetic leather for extracting marine facies, belong to conjunction Finished leather field.
Background technology
Superfine fiber chemical leather intensity is high, hydrolytic resistance is good, cold-resistant folding quality is excellent, skin emulation effect is strong, deep to receive market Welcome.The country quickly grew in recent years, was mainly used in the manufacture of sport footwear and high-grade sofa artificial leather, with technology content very high. Superfine fiber chemical leather is made by removing the marine facies in superfine fiber fabric again after superfine fiber fabric impregnation polyurethane resin Into.The minimizing technology of the marine facies in superfine fiber fabric mainly has two kinds of Toluene Extraction and Alkali reduction method.Toluene Extraction Woven fabric base fabric be made up of polyolefin and nylon 6, Toluene Extraction be first by superfine fiber fabric polyurethane resin be impregnated with, will The product being impregnated with is put into the DMF aqueous solution and solidifies, and then the washing of reusable heat water, DMF therein is cleaned up, then by product It is put into 80-95 DEG C of hot toluene solvent, repeatedly squeezing extraction, the polyolefin component that will be contained in superfine fiber fabric with toluene is molten Solution removal, is then washed away residual toluene with hot water, then dry and just obtain finished product.Toluene extraction process is most time-consuming in this technique Workshop section, superfine fiber fabric is coated completely mainly due to polyurethane after impregnation, surface is very fine and close so that toluene dissolve polyene Hydrocarbon and the polyolefin process of dissolution from base fabric become difficulty and the time is more long, have impact on production efficiency.
The content of the invention
The purpose of the present invention is to propose to a kind of preparation side of the easy polyurethane resin for superfine fiber synthetic leather for extracting marine facies Method, when being used to make superfine fiber chemical leather with polyurethane resin obtained in the method, can shorten toluene and extract polyolefin Time, improve production efficiency.
It is this it is easy extract marine facies the preparation method of polyurethane resin for superfine fiber synthetic leather be：By poly-dihydric alcohol, expand Chain agent is heated and reacted in a solvent with diisocyanate, antioxidant, catalyst, after being reacted to suitable viscosity, with end Only agent terminating reaction, adds other auxiliary agents, stirs, and obtains final products, wherein adding other to help after terminating reaction Be in mass raw material total amount 0.1%~10% water-soluble high-molecular material is additionally added while agent.
The preparation method of this easy polyurethane resin for superfine fiber synthetic leather for extracting marine facies of the invention is due to by water The macromolecular material of dissolubility is evenly spread in polyurethane solutions, and making superfine fibre with polyurethane resin obtained in the method closes During finished leather, during impregnation, water-soluble high-molecular material and polyurethane resin are coated on superfine fibre surface together, subsequent In hot water water-washing process, water-soluble high-molecular material and DMF are taken away by the water together, and very fine and close polyurethane surface was due to water originally The disengaging of soluble macromolecular and leave tiny micropore, it is ultra-fine that these micropores cause in extraction process toluene to be more easily accessible to Fiber base cloth, the polyolefin of dissolving is easier to be extracted, and accelerates the process of polyolefin component in dissolving removal base fabric, so that significantly Shorten the time that toluene extracts polyolefin.
Specific embodiment
It is this it is easy extract marine facies the preparation method of polyurethane resin for superfine fiber synthetic leather be：By poly-dihydric alcohol, expand Chain agent is heated and reacted in a solvent with diisocyanate, antioxidant, catalyst, after being reacted to corresponding viscosity, with end Only agent terminating reaction, adds other auxiliary agents, stirs, and obtains final products, wherein adding other to help after terminating reaction Be in mass raw material total amount 0.1%~10% water-soluble high-molecular material is additionally added while agent.
In the preparation method of this easy polyurethane resin for superfine fiber synthetic leather for extracting marine facies, described water solubility is high Molecular material can for polyethylene glycol, polyvinyl alcohol, carboxymethylcellulose calcium, hydroxypropyl methyl cellulose ether, polyacrylamide or One or more kinds of mixtures in polyvinylpyrrolidone.
Poly-dihydric alcohol in the preparation method of this easy polyurethane resin for superfine fiber synthetic leather for extracting marine facies can be with It is one or more the mixture in polyester diol, polyether Glycols or PCDL, poly-dihydric alcohol Number-average molecular weight is 1000~4000g/mol.
Diisocyanate in the preparation method of this easy polyurethane resin for superfine fiber synthetic leather for extracting marine facies can Think 4,4 '-methyl diphenylene diisocyanate, toluene di-isocyanate(TDI), different Buddhist diisocyanates, 4,4 '-dicyclohexyl One or more mixture in diisocyanate of the methane diisocyanate equimolecular quantity less than 300g/mol.
It is this it is easy extract marine facies polyurethane resin for superfine fiber synthetic leather preparation method in chain extender can be Molecular weight is glycol, diamines or the single methanol amine of 61~500g/mol.
Solvent in the preparation method of this easy polyurethane resin for superfine fiber synthetic leather for extracting marine facies can be two NMF.
Added after terminating reaction in the preparation method of this easy polyurethane resin for superfine fiber synthetic leather for extracting marine facies Other auxiliary agents can be antioxidant, ultraviolet absorber, weathering stabilizers, anti hydrolysis agent or antitack agent in one kind or two Plant the mixture of the above.The cooperation of these auxiliary agents and use ratio are being conducive to production to be smoothed out entering with synthetic leather final use Row selection.
Embodiment is described below.
Embodiment 1
Raw material proportioning：
Material name Quality (g)
MDI (4,4 '-methyl diphenylene diisocyanate) 100
Polyethylene glycol adipate glycol (number-average molecular weight 2000) 400
EG (ethylene glycol) 12.4
Catalyst：Stannous octoate 0.003
Antioxidant：Triphenyl phosphite 0.3
Solvent：Dimethylformamide (DMF) 1200
Auxiliary agent：BYK-333 (German BYK companies) 5
Methyl alcohol 1
Polyvinyl alcohol (Shanxi three-dimensional limited company) 50
Preparation process：
Polyalcohol polyethylene glycol adipate glycol 400g, antioxidant 0.3g, DMF600g are put into the reactor, plus Heat stirs 25min to 45 DEG C；Input MDI50g, kettle temperature control is reacted 1 hour at 75 DEG C, adds DMF400g, MDI30g, control 75 DEG C of reaction temperature processed continues to react, and as be added to remaining DMF in reactor by the growth of viscosity, puts into catalyst, and Remaining MDI is gradually added, until viscosity reaches 1.0 × 105mPa·s/25℃；Terminator methyl alcohol 1g reaction 60min are added, During polyvinyl alcohol 50g put into reactor, 70 DEG C of stirrings are uniformly dissolved discharging in 1 hour.
Embodiment 2
Raw material proportioning：
Material name Quality (g)
MDI (4,4 '-methyl diphenylene diisocyanate) 130.6
Polydiethylene glycol adipate glycol (number-average molecular weight 2000) 200
PCDL (molecular weight is 1000, and Japan produces) 200
Chain extender：1,4BG (1,4 butanediol) 20
Antioxidant：BHT, Shanghai lark company produces 0.2
Catalyst：Stannous octoate 0.007
Solvent：Dimethylformamide (DMF) 1300
Methyl alcohol 1
DC-193 (Dow Corning Corporation) 10
Carboxymethylcellulose calcium (Hua Wei celluloses Co., Ltd) 40
Polyethylene glycol (Jiangsu Hai'an Petrochemical Plant) 40
Preparation process：
PCDL, polydiethylene glycol adipate glycol, antioxidant, DMF500g are put into the reactor, 45 DEG C are heated to, and stir 25min；Input MDI50g, kettle temperature is controlled at 75 DEG C, and detection to reaction viscosity reaches 1.0 × 105mPa·s/25℃；After adding DMF400g and chain extender Isosorbide-5-Nitrae BG stirrings 30min, MDI50g is added to continue to react, temperature control System is reacted 1 hour at 75 DEG C；Input catalyst reaction 20min, progressively adds MDI, adds remaining DMF, then detects viscosity, Until viscosity reaches 2.4 × 105mPa·s/25℃；Add methyl alcohol and DC-193 reactions 30min.By carboxymethylcellulose calcium and poly- Ethylene glycol is added in reactor, is stirred, discharging.
Embodiment 3
Raw material proportioning：
Material name Quality (g)
MDI (4,4 '-methyl diphenylene diisocyanate) 73.4
TDI (toluene di-isocyanate(TDI), Shanghai Cohan wound) 31.3
PTMG (PolyTHF, molecular weight 2000, Hyosung group) 280
Polyadipate ethylene glycol butyl glycol ester diol (molecular weight 3000) 120
Chain extender：BDO 15
Chain extender：1,6 hexylene glycols 15
Antioxidant：BHT, Shanghai lark company produces 0.14
Catalyst：Stannous octoate 0.005
Solvent：DMF 1600
Methyl alcohol 1
DC-5043 (DOW CORNING) 50
Hydroxypropyl methyl cellulose ether (Shandong Fu Ying bio tech ltd) 100
Preparation process：
Input PTMG, polyadipate ethylene glycol butyl glycol ester diol, antioxidant, DMF200g, are heated in the reactor 45 DEG C, and stir 25min；Input TDI31.3g, kettle temperature is controlled at 80 DEG C, and detection to reaction viscosity reaches 1.2 × 105mPa· s/25℃；Add DMF800g and chain extender；After stirring 30min, MDI55g is added to continue to react, temperature control is reacted at 75 DEG C 1 hour；Input catalyst reaction 20min, progressively adds MDI, adds remaining DMF, then detects viscosity, until viscosity reaches 1.8×105mPa·s/25℃；Methyl alcohol and DC-5043 reaction 40min are added, then hydroxypropyl methyl cellulose ether is put into instead In answering device, after stirring 1h, the discharging to after being uniformly dispersed.
Embodiment 4
Raw material proportioning：
Material name Quality (g)
MDI (4,4 '-methyl diphenylene diisocyanate) 132.7
Polypropylene oxide glycol (molecular weight 2000, national capital Chemical Co., Ltd.) 220
Polyneopentyl glycol adipate glycol (molecular weight 2000) 180
Chain extender：EG 15
Chain extender：1,2-PD 8
Antioxidant：BHT (Shanghai lark company product) 0.14
Catalyst：Dibutyl tin dilaurate 0.0005
Solvent：DMF 2500
Methyl alcohol 1
DC-1248 (DOW CORNING) 20
Carboxymethylcellulose calcium (Hua Wei celluloses Co., Ltd) 25
Polyvinyl alcohol (Shanxi three-dimensional limited company) 25
Preparation process：
Input polyalcohol, antioxidant, DMF500g, are heated to 45 DEG C, and stir 25min in the reactor；Input MDI100g, kettle temperature control stirs 2h at 75 DEG C；After stirring 30min after addition DMF500g and chain extender, MDI20g is added to continue Reaction, temperature control is reacted 1 hour at 75 DEG C；Input catalyst reaction 20min, progressively adds MDI, adds remaining DMF, Viscosity is detected again, until viscosity reaches 1.0 × 105mPa·s/25℃；After adding methyl alcohol, DC-1248 reactions 60min, then by carboxylic Discharging after methylcellulose and polyvinyl alcohol addition.
Embodiment 5
Raw material proportioning：
Preparation process：
Input polyalcohol, antioxidant, catalyst, DMF400g, are heated to 45 DEG C, and stir 25min in the reactor； Input isophorone diisocyanate 60g, kettle temperature control reaches 1.2 × 10 in 95 DEG C of reactions, detection to reaction viscosity5mPa·s/ 25℃；After stirring 30min after addition DMF800g and chain extender, MDI80g is added to continue to react, temperature control reacts 1 at 80 DEG C Hour；Input catalyst reaction 20min, progressively adds MDI, adds remaining DMF, then detects viscosity, until viscosity reaches 1.8 ×105mPa·s/25℃；Methyl alcohol, DC-L5309 reaction 90min are added, polyethylene glycol and polyvinyl alcohol is added, 1h is to molten for stirring Solution is uniform, discharging.
Embodiment 6
Raw material proportioning：
Material name Quality (g)
MDI (4,4 '-methyl diphenylene diisocyanate) 88.5
4,4 '-dicyclohexyl methyl hydride diisocyanate (Degussa) 50
PTMG (molecular weight 1000, Japan produces) 100
Polycaprolactone diols (molecular weight 2000, Shenzhen brilliance great achievement limited company) 300
Chain extender：MEA (MEA) 18
Antioxidant：BHT, Shanghai lark company produces 0.5
Catalyst：Stannous octoate 0.05
Solvent：DMF 1150
Propyl alcohol 1.5
BYK-LPG7018 20
DC-1248 40
Carboxymethylcellulose calcium (Hua Wei celluloses Co., Ltd) 100
Polyvinylpyrrolidone (Nanjing Rui Ze Fine Chemical Co., Ltd) 50
Preparation process：
Input polyalcohol, antioxidant, catalyst, chain extender and DMF500g, are heated to 45 DEG C, and stir in the reactor Mix 25min；Input 4,4 '-dicyclohexyl methyl hydride diisocyanate 50g；Kettle temperature is controlled at 90 DEG C, after reacting 1.5 hours, is added After DMF300g stirrings 30min, MDI70g is added to continue to react, temperature control is reacted 1 hour at 70 DEG C；MDI is progressively added, plus Enter remaining DMF, then detect viscosity, until viscosity reaches 1.5 × 105mPa·s/25℃；Add propyl alcohol, BYK-LPG7018, DC-1248 reacts 60min, adds carboxymethylcellulose calcium and polyvinylpyrrolidone, stirring 1h to uniform, discharging.
Embodiment 7
Raw material proportioning：
Preparation process：
Input polyalcohol, antioxidant, catalyst, chain extender DMF600g, are heated to 45 DEG C, and stir in the reactor 25min；Input MDI110g, kettle temperature is controlled at 80 DEG C, reacts 60min；DMF800g and MDI60g is added to continue to react, temperature control System is reacted 1 hour at 80 DEG C；Progressively add MDI, add remaining DMF, then detect viscosity, 1.4 are reached until viscosity × 105mPa·s/25℃；Ethanol, DC-1990 and BYK-LPX20192 reaction 60min are added, polyacrylamide and poly- second is added Enol, 60min is to being uniformly dispersed for stirring, discharging.
With under the formulation condition same with early stage of the resin prepared by above-described embodiment, the later stage be added without water soluble polymer close Into resin；After same process conditions have been impregnated with woven fabric base fabric, the time contrast that contrast toluene extracts polyolefin is as follows：
Embodiment 1 2 3 4 5 6 7
It is not added with water soluble polymer 71min 68min 79min 85min 81min 81min 81min
Add water soluble polymer 48min 43min 43min 55min 38min 40min 41min
As seen from the above table, can greatly improve toluene with resin obtained in the inventive method, after impregnation woven fabric and extract polyene The speed of hydrocarbon, improves production efficiency.

Claims (7)

1. it is a kind of it is easy extract marine facies polyurethane resin for superfine fiber synthetic leather preparation method, by poly-dihydric alcohol, chain extender Heated in a solvent with diisocyanate, antioxidant, catalyst and reacted, after being reacted to suitable viscosity, use terminator Terminating reaction, adds other auxiliary agents, stirs, and obtains final products, it is characterised in that add other after terminating reaction Be in mass raw material total amount 0.1%~10% water-soluble high-molecular material is additionally added while auxiliary agent.
2. the preparation method of the polyurethane resin for superfine fiber synthetic leather of marine facies is easily extracted as claimed in claim 1, and it is special Levy is that described water-soluble high-molecular material is polyethylene glycol, polyvinyl alcohol, carboxymethylcellulose calcium, hydroxypropyl methyl cellulose One or more kinds of mixtures in ether, polyacrylamide, polyvinylpyrrolidone.
3. the preparation method of the polyurethane resin for superfine fiber synthetic leather of marine facies is easily extracted as claimed in claim 1 or 2, its Be characterised by described poly-dihydric alcohol in polyester diol, polyether Glycols and PCDL one or two with On mixture, the number-average molecular weight of poly-dihydric alcohol is 1000~4000g/mol.
4. the preparation method of the polyurethane resin for superfine fiber synthetic leather of marine facies is easily extracted as claimed in claim 3, and it is special It is one or more mixed in diisocyanate of the described diisocyanate for molecular weight less than 300g/mol to levy Compound.
5. the preparation method of the polyurethane resin for superfine fiber synthetic leather of marine facies is easily extracted as claimed in claim 4, and it is special Levy glycol, diamines or single methanol amine that the chain extender described in being is 61~500g/mol of molecular weight.
6. the preparation method of the polyurethane resin for superfine fiber synthetic leather of marine facies is easily extracted as claimed in claim 5, and it is special Levy is that described solvent is dimethylformamide.
7. the preparation method of the polyurethane resin for superfine fiber synthetic leather of marine facies is easily extracted as claimed in claim 6, and it is special It is surfactant, antioxidant, ultraviolet absorber, weather-stable to levy other auxiliary agents added after the terminating reaction described in being One or more kinds of mixtures in agent, anti hydrolysis agent and antitack agent.
CN201710191593.8A 2017-03-28 2017-03-28 Easily extract the preparation method of the polyurethane resin for superfine fiber synthetic leather of marine facies Pending CN106866916A (en)

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