CN101368337B - Function adjuvant for improving sanitation performance of superfine fibre chemical leather and preparation method thereof - Google Patents
Function adjuvant for improving sanitation performance of superfine fibre chemical leather and preparation method thereof Download PDFInfo
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- CN101368337B CN101368337B CN2008102317364A CN200810231736A CN101368337B CN 101368337 B CN101368337 B CN 101368337B CN 2008102317364 A CN2008102317364 A CN 2008102317364A CN 200810231736 A CN200810231736 A CN 200810231736A CN 101368337 B CN101368337 B CN 101368337B
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Abstract
The invention relates to a method to prepare functional addition agent for synthesizing leather, in particular relates to functional addition agent used for improving the hygienic property of synthesized ultra-thin fiber leather and a preparation method thereof. The invention aims at solving the problem of poor hygienic property of synthesized ultra-thin fiber leather in the prior art; the technical proposal provided by the invention includes that: the functional addition agent used for improving the hygienic property of synthesized ultra-thin fiber leather is prepared through the following steps: firstly, mixing: mixing alcohol amine and acrylate, adding proper amount of low fatty alcohol as solvent, so as to enable the mixture to react, then removing the solvent under decompressed condition for spare use; secondly, catalyzing: adding acid catalyzer for acid catalysis, pumping to vacuum and enabling the mixture to react, thus producing hydroxyl-terminated hyperbranched polyamido ester. Compared with the prior art, the method has the advantages that the product produced through the method is large in degree of functionality and high in reaction activity and can be combined with active groups, with water permeability and moisture absorption capability both improved by 30%.
Description
Technical field:
That the present invention relates to is the preparation method of synthetic leather function additive, is specifically related to a kind of function additive that improves sanitation performance of superfine fibre chemical leather and preparation method thereof.
Background technology
Superfine fiber chemical leather exactly likes corium on structure and performance, main feature and advantage that it has are as follows: 1. be fit to large-scale continuous industrial production; 2. the formation of bundle superfine fibre and continuous reticulated polyurethane structure make it have structure and the feel of part near natural leather; 3. physical and chemical performance excellence.All be better than natural leather at aspects such as mechanical strength, water-fast, oil resistant, weatherabilities, be particularly suitable under adverse circumstances and high strength, high humility, large amount of exercise condition, using; 4. manufacturing process is various, and designs and varieties are various; 5. removing from office the body homogeneous, not have the position poor, on thickness, can adjust freely, adapt to the needs of multiple product, its use can effectively improve the class and the added value of product, thereby has application widely in industries such as military project, labour protection, shoemaking, case and bag, furniture, clothes and sports equipments.
But the shortcoming that it exists also clearly, because the active group on the superfine fiber fabric seldom, compare with protein fibre, only have its about 10%, therefore the fatal shortcoming of superfine fiber chemical leather be exactly its sanitation performance (gas permeability, water vapor permeability and hygroscopicity) far away than corium difference, so its scope of application is restricted to a certain extent.
Improve the sanitation performance of superfine fiber chemical leather, just need to improve the active group on the superfine fiber fabric, but at present in the preparation field of the function additive that improves sanitation performance of superfine fibre chemical leather, it is available still not have ripe industrial products.
Summary of the invention
The purpose of this invention is to provide a kind of function additive that improves sanitation performance of superfine fibre chemical leather and preparation method thereof, to solve the problem of the sanitation performance of superfine fibre chemical leather difference that prior art exists.
For solving the problem that prior art exists, technical scheme of the present invention is: a kind of function additive that improves sanitation performance of superfine fibre chemical leather, made by following preparation method: this preparation method comprises the steps: successively
One, mix: at first hydramine is mixed by the mol ratio of 1:1～3 with acrylate, add an amount of low carbon chain fatty alcohol as solvent, behind 10～60 ℃ of following stirring reaction 1～7h, removal of solvent under reduced pressure, standby;
Two, catalysis: 3%～7% the acidic catalyst that adds the reactant gross mass carries out acidic catalyst, vacuumizes under 100～150 ℃, and vacuum is 0.02～0.1MPa, and reaction 1～5h makes superbrnaching end-hydroxy polyamide-ester.
Such scheme also comprises modification procedure, in this step: is the mixed in molar ratio of 1～4:1 with superbrnaching end-hydroxy polyamide-ester and dicarboxylic anhydride by the hydroxyl and the acid anhydrides of superbrnaching end-hydroxy polymer, 1%～5% the acidic catalyst that adds the reactant gross mass, at 70～100 ℃ of following stirring reaction 1～3h, make.
The aforesaid propylene acid esters is a methyl acrylate, ethyl acrylate or butyl acrylate; Hydramine is diethanol amine or diisopropanolamine (DIPA); Low carbon chain fatty alcohol is an absolute methanol, absolute ethyl alcohol or anhydrous isopropyl alcohol; Acidic catalyst is the concentrated sulfuric acid, p-methyl benzenesulfonic acid or dry HCl; Dicarboxylic anhydride is maleic anhydride or succinic anhydride.
A kind of preparation method who improves the function additive of sanitation performance of superfine fibre chemical leather comprises the steps successively
One, mix: at first hydramine is mixed by the mol ratio of 1:1～3 with acrylate, add an amount of low carbon chain fatty alcohol as solvent, behind 10～60 ℃ of following stirring reaction 1～7h, removal of solvent under reduced pressure, standby;
Two, catalysis: 3%～7% the acidic catalyst that adds the reactant gross mass carries out acidic catalyst, vacuumizes under 100～150 ℃, and vacuum is 0.02～0.1MPa, and reaction 1～5h makes superbrnaching end-hydroxy polyamide-ester.
Such scheme also comprises modification procedure, in this step: is the mixed in molar ratio of 1～4:1 with superbrnaching end-hydroxy polyamide-ester and dicarboxylic anhydride by the hydroxyl and the acid anhydrides of superbrnaching end-hydroxy polymer, 1%～5% the acidic catalyst that adds the reactant gross mass, at 70～100 ℃ of following stirring reaction 1～3h, make.
The aforesaid propylene acid esters is a methyl acrylate, ethyl acrylate or butyl acrylate; Hydramine is diethanol amine or diisopropanolamine (DIPA); Low carbon chain fatty alcohol is an absolute methanol, absolute ethyl alcohol or anhydrous isopropyl alcohol; Acidic catalyst is the concentrated sulfuric acid, p-methyl benzenesulfonic acid or dry HCl; Dicarboxylic anhydride is maleic anhydride or succinic anhydride.
Compared with prior art, advantage of the present invention is as follows: the synthetic leather auxiliary agent end-group functionality of this method preparation is big, the reactivity height, can combine with the active group on the synthetic fiber molecule, significantly improve the water vapor permeability and the hygroscopicity of superfine fiber chemical leather, water vapor permeability and hygroscopicity all can improve 30%.
Description of drawings:
Fig. 1: the synthetic reaction formula of methyl acrylate and diethanol amine;
Fig. 2: the synthetic reaction formula of superbrnaching end-hydroxy poly-(amide-ester).
The specific embodiment:
Below in conjunction with accompanying drawing the present invention is elaborated.
Embodiment 1:
A kind of function additive that improves sanitation performance of superfine fibre chemical leather, made by following preparation method: this preparation method comprises the steps successively
Step 1: diethanol amine is mixed by the mol ratio of 1:1 with methyl acrylate, add the 20mL absolute methanol, behind 35 ℃ of following stirring reaction 4h,, vacuumize except that after desolvating with the product of gained as solvent, standby;
Step 2: 4% the p-methyl benzenesulfonic acid that adds the reactant gross mass carries out acidic catalyst, vacuumizes (vacuum is 0.05MPa) reaction 3h under 120 ℃, makes superbrnaching end-hydroxy polyamide-ester.
Embodiment 2:
A kind of function additive that improves sanitation performance of superfine fibre chemical leather, made by following preparation method: this preparation method comprises the steps successively
Step 1: diisopropanolamine (DIPA) is mixed by the mol ratio of 1:1.5 with ethyl acrylate, adds the 30mL absolute ethyl alcohol, behind 30 ℃ of following stirring reaction 5h, the product of gained is directly moved into Dewar bottle as solvent, vacuumize remove desolvate after, standby:
Step 2: the concentrated sulfuric acid that adds reactant gross mass 3% carries out acidic catalyst, vacuumizes (vacuum is 0.1MPa) reaction 2h under 130 ℃, makes superbrnaching end-hydroxy polyamide-ester.
Embodiment 3:
A kind of function additive that improves sanitation performance of superfine fibre chemical leather, made by following preparation method: this preparation method comprises the steps successively
Step 1: diethanol amine is mixed by the mol ratio of 1:2.5 with butyl acrylate, add the 35mL anhydrous isopropyl alcohol as solvent, behind 40 ℃ of following stirring reaction 3h, the product of gained removes and desolvates, and is standby:
Step 2: the dry HCl that adds reactant gross mass 3% carries out acidic catalyst, vacuumizes (vacuum is 0.08MPa) reaction 2.5h under 130 ℃, makes superbrnaching end-hydroxy polyamide-ester;
Step 3: with the mixed in molar ratio that the hydroxyl in superbrnaching end-hydroxy polyamide-ester and maleic anhydride are pressed 2.1:1, add mass percent and be 3% p-methyl benzenesulfonic acid, get final product at 180 ℃ of following stirring reaction 2.5h.
Embodiment 4:
A kind of function additive that improves sanitation performance of superfine fibre chemical leather, made by following preparation method: this preparation method comprises the steps successively
One, mix: at first diethanol amine is mixed by the mol ratio of 1:1.1 with methyl acrylate, the absolute methanol of adding 35mL is as solvent, behind 40 ℃ of following stirring reaction 3h, and removal of solvent under reduced pressure, standby;
Two, catalysis: 3% the concentrated sulfuric acid that adds the reactant gross mass carries out acidic catalyst, vacuumizes (vacuum is 0.04MPa) reaction 1h under 130 ℃, makes superbrnaching end-hydroxy polyamide-ester;
Three, modification: is the mixed in molar ratio of 2.1:1 with superbrnaching end-hydroxy polyamide-ester and maleic anhydride by the hydroxyl and the acid anhydrides of superbrnaching end-hydroxy polymer, adds 3% the concentrated sulfuric acid of reactant gross mass, at 80 ℃ of following stirring reaction 2.5h, makes.
Embodiment 5:
A kind of function additive that improves sanitation performance of superfine fibre chemical leather, made by following preparation method: this preparation method comprises the steps successively
One, mix: at first diisopropanolamine (DIPA) is mixed by the mol ratio of 1:3 with ethyl acrylate, the absolute ethyl alcohol of adding 40mL is as solvent, behind 60 ℃ of following stirring reaction 7h, and removal of solvent under reduced pressure, standby;
Two, catalysis: 7% the p-methyl benzenesulfonic acid that adds the reactant gross mass carries out acidic catalyst, vacuumizes (vacuum is 0.1MPa) reaction 5h under 150 ℃, makes superbrnaching end-hydroxy polyamide-ester;
Three, modification: is the mixed in molar ratio of 4:1 with superbrnaching end-hydroxy polyamide-ester and maleic anhydride by the hydroxyl and the acid anhydrides of superbrnaching end-hydroxy polymer, adds 5% p-methyl benzenesulfonic acid of reactant gross mass, at 100 ℃ of following stirring reaction 3h, makes.
Embodiment 6:
A kind of function additive that improves sanitation performance of superfine fibre chemical leather, made by following preparation method: this preparation method comprises the steps successively
One, mix: at first diisopropanolamine (DIPA) is mixed by the mol ratio of 1:2 with butyl acrylate, the anhydrous isopropyl alcohol of adding 30mL is as solvent, behind 10 ℃ of following stirring reaction 1h, and removal of solvent under reduced pressure, standby;
Two, catalysis: the HCl that adds 4% drying of reactant gross mass carries out acidic catalyst, vacuumizes (vacuum is 0.02MPa) reaction 3h under 100 ℃, makes superbrnaching end-hydroxy polyamide-ester;
Three, modification: with superbrnaching end-hydroxy polyamide-ester and succinic anhydride, be the mixed in molar ratio of 1:1, add the HCl of 1% drying of reactant gross mass,, make at 70 ℃ of following stirring reaction 1h by the hydroxyl and the acid anhydrides of superbrnaching end-hydroxy polymer.
Claims (4)
1. function additive that improves sanitation performance of superfine fibre chemical leather, made by following preparation method: this preparation method comprises the steps successively
One, mix: at first hydramine is mixed by 1: 1～3 mol ratio with acrylate, add an amount of low carbon chain fatty alcohol as solvent, behind 10～60 ℃ of following stirring reaction 1～7h, removal of solvent under reduced pressure, standby;
Two, catalysis: 3%～7% the acidic catalyst that adds the reactant gross mass carries out acidic catalyst, vacuumizes under 100～150 ℃, and vacuum is 0.02～0.1MPa, and reaction 1～5h makes superbrnaching end-hydroxy polyamide-ester, it is characterized in that:
Described method also comprises modification procedure, in this step: be 1～4: 1 mixed in molar ratio with superbrnaching end-hydroxy polyamide-ester and dicarboxylic anhydride by the hydroxyl of superbrnaching end-hydroxy polymer and acid anhydrides, 1%～5% the acidic catalyst that adds the reactant gross mass, at 70～100 ℃ of following stirring reaction 1～3h, make.
2. the function additive of raising sanitation performance of superfine fibre chemical leather as claimed in claim 1 is characterized in that: described acrylate is a methyl acrylate, ethyl acrylate or butyl acrylate; Hydramine is diethanol amine or diisopropanolamine (DIPA); Low carbon chain fatty alcohol is an absolute methanol, absolute ethyl alcohol or anhydrous isopropyl alcohol; Acidic catalyst is the concentrated sulfuric acid, p-methyl benzenesulfonic acid or dry HCl; Dicarboxylic anhydride is maleic anhydride or succinic anhydride.
3. the preparation method of the function additive of raising sanitation performance of superfine fibre chemical leather as claimed in claim 1 comprises the steps: successively
One, mix: at first hydramine is mixed by 1: 1～3 mol ratio with acrylate, add an amount of low carbon chain fatty alcohol as solvent, behind 10～60 ℃ of following stirring reaction 1～7h, removal of solvent under reduced pressure, standby;
Two, catalysis: 3%～7% the acidic catalyst that adds the reactant gross mass carries out acidic catalyst, vacuumizes under 100～150 ℃, and vacuum is 0.02～0.1MPa, and reaction 1～5h makes superbrnaching end-hydroxy polyamide-ester, it is characterized in that:
Described method also comprises modification procedure, in this step: be 1～4: 1 mixed in molar ratio with superbrnaching end-hydroxy polyamide-ester and dicarboxylic anhydride by the hydroxyl of superbrnaching end-hydroxy polymer and acid anhydrides, 1%～5% the acidic catalyst that adds the reactant gross mass, at 70～100 ℃ of following stirring reaction 1～3h, make.
4. the preparation method of the function additive of raising sanitation performance of superfine fibre chemical leather as claimed in claim 3 is characterized in that: described acrylate is a methyl acrylate, ethyl acrylate or butyl acrylate; Hydramine is diethanol amine or diisopropanolamine (DIPA); Low carbon chain fatty alcohol is an absolute methanol, absolute ethyl alcohol or anhydrous isopropyl alcohol; Acidic catalyst is the concentrated sulfuric acid, p-methyl benzenesulfonic acid or dry HCl; Dicarboxylic anhydride is maleic anhydride or succinic anhydride.
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| CN101368337B true CN101368337B (en) | 2011-01-26 |
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| CN101956333B (en) * | 2010-08-25 | 2013-01-09 | 厦门泓信超细纤维材料有限公司 | Method for improving hygienic performance of figured-island superfine fiber synthetic leather |
| CN102140763B (en) * | 2011-01-29 | 2012-10-17 | 陕西科技大学 | After finishing method for permanently improving hygiene performance of superfine fiber synthetic leather base cloth |
| CN102493194B (en) * | 2011-12-09 | 2013-12-04 | 陕西科技大学 | Method for modifying superfine fiber synthetic leather based on amino-terminated hyperbranched polymer |
| CN103184692B (en) * | 2013-04-11 | 2015-02-18 | 济南大学 | Application of hyperbranched polymer in belt core interface agent of flame-retardant conveying belt |
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