CN105440251A - Preparation method of carboxylate acetate fiber emulsion - Google Patents
Preparation method of carboxylate acetate fiber emulsion Download PDFInfo
- Publication number
- CN105440251A CN105440251A CN201510872908.6A CN201510872908A CN105440251A CN 105440251 A CN105440251 A CN 105440251A CN 201510872908 A CN201510872908 A CN 201510872908A CN 105440251 A CN105440251 A CN 105440251A
- Authority
- CN
- China
- Prior art keywords
- cellulose acetate
- preparation
- carboxylic acid
- acid type
- cooled
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
- C08G18/75—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic
- C08G18/751—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring
- C08G18/752—Polyisocyanates 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
- C08G18/753—Polyisocyanates 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
- C08G18/755—Polyisocyanates 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/04—Acids; Metal salts or ammonium salts thereof
- C08F220/06—Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/26—Esters containing oxygen in addition to the carboxy oxygen
- C08F220/28—Esters containing oxygen in addition to the carboxy oxygen containing no aromatic rings in the alcohol moiety
-
- 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
- C08G18/4009—Two or more macromolecular compounds not provided for in one single group of groups C08G18/42 - C08G18/64
- C08G18/4081—Mixtures of compounds of group C08G18/64 with other macromolecular compounds
-
- 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
- C08G18/62—Polymers of compounds having carbon-to-carbon double bonds
- C08G18/6216—Polymers of alpha-beta ethylenically unsaturated carboxylic acids or of derivatives thereof
- C08G18/625—Polymers of alpha-beta ethylenically unsaturated carboxylic acids; hydrolyzed polymers of esters of these acids
- C08G18/6254—Polymers of alpha-beta ethylenically unsaturated carboxylic acids and of esters of these acids containing 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
- 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
- C08G18/64—Macromolecular compounds not provided for by groups C08G18/42 - C08G18/63
- C08G18/6484—Polysaccharides and derivatives thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/26—Esters containing oxygen in addition to the carboxy oxygen
- C08F220/28—Esters containing oxygen in addition to the carboxy oxygen containing no aromatic rings in the alcohol moiety
- C08F220/281—Esters containing oxygen in addition to the carboxy oxygen containing no aromatic rings in the alcohol moiety and containing only one oxygen, e.g. furfuryl (meth)acrylate or 2-methoxyethyl (meth)acrylate
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2375/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
- C08J2375/04—Polyurethanes
Abstract
The invention discloses a preparation method of a carboxylate acetate fiber emulsion. The preparation method comprises the following steps: weighing acrylic acid, hydroxyethyl acrylate, butanone and recrystallized azodiisobutyronitrile; adding acrylic acid, hydroxyethyl acrylate and butanone into a flask; adding recrystallized azodiisobutyronitrile; stirring for reaction under a 70 to 78 DEG C thermostatic condition; reducing the temperature to 40 to 55 DEG C; adding dibutyltin dilaurate and isophorone diisocyanate; carrying out thermostatic stirring for reaction; heating to 50 to 70 DEG C; adding acetate fiber dissolved with methyl acetate; carrying out a heat-insulating reaction; reducing the temperature to 35 to 55 DEG C; adding triethylamine; carrying out heat-insulating salifying; reducing the temperature to 20 to 40 DEG C; adding deionized water; stirring; carrying out heat-insulating dispersing to obtain the carboxylate acetate fiber emulsion. The carboxylate acetate fiber emulsion prepared according to the preparation method is relatively high in stability and dispersity.
Description
Technical field
The present invention relates to a kind of preparation method of fibre emulsion, be specifically related to a kind of preparation method of carboxylic acid type cellulose acetate emulsion.
Background technology
Cellulose ethanoate, i.e. cellulose acetate (CA), be take acetic acid as solvent, aceticanhydride is acetylizing agent, through a kind of thermoplastic resin that esterification obtains; Carry out merchandized handling the earliest in derivatived cellulose, and the cellulose organic ester of development.It has that crushing resistance is strong, excellent touch, selectivity are high, permeable amount is large, flame resistivity and anti-acid is strong, processing simply and the feature such as reusable edible.Therefore be applied to the aspects such as handle for tool, toy, tableware hand handle, photo egative film, also can be used as the composition of some sizing agent simultaneously.In recent years, due to the increase of environmental stress, solvent-borne type cellulose ester analog derivative product is replaced by the environment-friendly type aqueous cellulose ester series products with water by medium gradually.At present, for the Water-borne modification research of cellulose substances, usually be research object with nitrocotton, and the development for coating and sizing agent industry is provided a new approach by the Water-borne modification of cellulose acetate, but existing cellulose acetate stability of emulsion and dispersed poor.
Summary of the invention
The object of the invention is to the shortcoming overcoming above-mentioned prior art, provide a kind of preparation method of carboxylic acid type cellulose acetate emulsion, this carboxylic acid type cellulose acetate emulsion intercalation method and dispersiveness are better.
For achieving the above object, the preparation method of carboxylic acid type cellulose acetate emulsion of the present invention comprises the following steps:
Take vinylformic acid, Hydroxyethyl acrylate, the Diisopropyl azodicarboxylate of butanone and recrystallization, again by vinylformic acid, Hydroxyethyl acrylate and butanone join in flask, then the Diisopropyl azodicarboxylate of recrystallization is added, constant temperature stirring reaction under the condition of 70-78 DEG C, dibutyl tin laurate and isophorone diisocyanate is added after being cooled to 40-55 DEG C, and carry out constant temperature stirring reaction, be warming up to 50-70 DEG C again, then the cellulose acetate that methyl acetate dissolves is added, 35-55 DEG C is cooled to after insulation reaction, add triethylamine again, 20-40 DEG C is cooled to after insulation salify, then deionized water is added, carry out stirring insulation dispersion again, obtain carboxylic acid type cellulose acetate emulsion.
The ratio of cellulose acetate, triethylamine and deionized water that the Diisopropyl azodicarboxylate of described vinylformic acid, Hydroxyethyl acrylate, butanone, recrystallization, dibutyl tin laurate, isophorone diisocyanate, methyl acetate dissolve is 1.0-8g:0.5-6.0g:10-30g:0.1-1g:0.1-0.8g:1.0-8.0g:1.0-6.0g: 1.0-9.0g:60ml.
Under the condition of 70-78 DEG C constant temperature stirring reaction process in the speed that stirs be 200rpm, the reaction times is 1.5h.
The dibutyl tin laurate after the process of 4A molecular sieve dehydration and isophorone diisocyanate is added after being cooled to 40-55 DEG C.
Dibutyl tin laurate and isophorone diisocyanate is added after being cooled to 40-55 DEG C, and constant temperature stirring reaction 1h, wherein, the speed of stirring is 400rpm.
35-55 DEG C is cooled to after insulation reaction 2h.
Stirring the speed stirred in the process of insulation dispersion is 2000rpm, and the time of insulated and stirred dispersion is 30min.
The present invention has following beneficial effect:
The preparation method of carboxylic acid type cellulose acetate emulsion of the present invention is in preparation process, using the Diisopropyl azodicarboxylate of recrystallization (AIBN) as initiator, and using vinylformic acid as hydrophilic component, vinylformic acid and Hydroxyethyl acrylate is utilized to be-the OH that raw material prepares in preliminary performed polymer, then-the OH in preliminary performed polymer is polymerized with the isocyanate group (-NCO) in isophorone diisocyanate respectively with the-OH in cellulose acetate, after triethylamine salify, add deionized water emulsification again, thus prepare carboxylic acid type cellulose acetate emulsion.In preparation process, hydrophilic radical is incorporated in cellulosic polymer chain by the interaction by Hydroxyethyl acrylate (HEMA), isoflurane chalcone diisocyanate (IPDI) and cellulose acetate (CA), thus make the carboxylic acid type cellulose acetate emulsion of preparation have good stability and dispersiveness, and environment friendly and pollution-free.
Embodiment
Being described in further detail the present invention below in conjunction with specific embodiment, is below explanation of the invention instead of restriction.
Embodiment one
The preparation method of carboxylic acid type cellulose acetate emulsion of the present invention comprises the following steps:
Take vinylformic acid, Hydroxyethyl acrylate, the Diisopropyl azodicarboxylate of butanone and recrystallization, again by vinylformic acid, Hydroxyethyl acrylate and butanone join in flask, then the Diisopropyl azodicarboxylate of recrystallization is added, constant temperature under the condition of 78 DEG C be 200rpm stirring reaction 1.5h with speed, the dibutyl tin laurate after the process of 4A molecular sieve dehydration and isophorone diisocyanate is added after being cooled to 40 DEG C, and carry out constant temperature stirring reaction 1h, wherein, stirring velocity is 400rpm, be warming up to 50 DEG C again, then the cellulose acetate that methyl acetate dissolves is added, 35 DEG C are cooled to after insulation reaction 2h, add triethylamine again, 20 DEG C are cooled to after insulation salify, then deionized water is added, be that 2000rpm stirs insulation dispersion 30min again with stirring velocity, obtain carboxylic acid type cellulose acetate emulsion,
The ratio of cellulose acetate, triethylamine and deionized water that the Diisopropyl azodicarboxylate of described vinylformic acid, Hydroxyethyl acrylate, butanone, recrystallization, dibutyl tin laurate, isophorone diisocyanate, methyl acetate dissolve is 1.0g:6.0g:10g:1g:0.1g:8.0g:1.0g:9.0g:60ml.
Embodiment two
The preparation method of carboxylic acid type cellulose acetate emulsion of the present invention comprises the following steps:
Take vinylformic acid, Hydroxyethyl acrylate, the Diisopropyl azodicarboxylate of butanone and recrystallization, again by vinylformic acid, Hydroxyethyl acrylate and butanone join in flask, then the Diisopropyl azodicarboxylate of recrystallization is added, constant temperature under the condition of 70 DEG C be 200rpm stirring reaction 1.5h with speed, the dibutyl tin laurate after the process of 4A molecular sieve dehydration and isophorone diisocyanate is added after being cooled to 55 DEG C, and carry out constant temperature stirring reaction 1h, wherein, stirring velocity is 400rpm, be warming up to 70 DEG C again, then the cellulose acetate that methyl acetate dissolves is added, 55 DEG C are cooled to after insulation reaction 2h, add triethylamine again, 40 DEG C are cooled to after insulation salify, then deionized water is added, be that 2000rpm stirs insulation dispersion 30min again with stirring velocity, obtain carboxylic acid type cellulose acetate emulsion,
The ratio of cellulose acetate, triethylamine and deionized water that the Diisopropyl azodicarboxylate of described vinylformic acid, Hydroxyethyl acrylate, butanone, recrystallization, dibutyl tin laurate, isophorone diisocyanate, methyl acetate dissolve is 8g:0.5g:30g:0.1g:0.8g:1.0g:6.0g:1.0g:60ml.
Embodiment three
The preparation method of carboxylic acid type cellulose acetate emulsion of the present invention comprises the following steps:
Take vinylformic acid, Hydroxyethyl acrylate, the Diisopropyl azodicarboxylate of butanone and recrystallization, again by vinylformic acid, Hydroxyethyl acrylate and butanone join in flask, then the Diisopropyl azodicarboxylate of recrystallization is added, constant temperature under the condition of 75 DEG C be 200rpm stirring reaction 1.5h with speed, the dibutyl tin laurate after the process of 4A molecular sieve dehydration and isophorone diisocyanate is added after being cooled to 50 DEG C, and carry out constant temperature stirring reaction 1h, wherein, stirring velocity is 400rpm, be warming up to 60 DEG C again, then the cellulose acetate that methyl acetate dissolves is added, 40 DEG C are cooled to after insulation reaction 2h, add triethylamine again, 30 DEG C are cooled to after insulation salify, then deionized water is added, be that 2000rpm stirs insulation dispersion 30min again with stirring velocity, obtain carboxylic acid type cellulose acetate emulsion,
The ratio of cellulose acetate, triethylamine and deionized water that the Diisopropyl azodicarboxylate of described vinylformic acid, Hydroxyethyl acrylate, butanone, recrystallization, dibutyl tin laurate, isophorone diisocyanate, methyl acetate dissolve is 5g:3g:20g:0.5g:0.5g:5g:3g:5g:60ml.
Embodiment four
The preparation method of carboxylic acid type cellulose acetate emulsion of the present invention comprises the following steps:
Take vinylformic acid, Hydroxyethyl acrylate, the Diisopropyl azodicarboxylate of butanone and recrystallization, again by vinylformic acid, Hydroxyethyl acrylate and butanone join in flask, then the Diisopropyl azodicarboxylate of recrystallization is added, constant temperature under the condition of 75 DEG C be 200rpm stirring reaction 1.5h with speed, the dibutyl tin laurate after the process of 4A molecular sieve dehydration and isophorone diisocyanate is added after being cooled to 45 DEG C, and carry out constant temperature stirring reaction 1h, wherein, stirring velocity is 400rpm, be warming up to 55 DEG C again, then the cellulose acetate that methyl acetate dissolves is added, 40 DEG C are cooled to after insulation reaction 2h, add triethylamine again, 25 DEG C are cooled to after insulation salify, then deionized water is added, be that 2000rpm stirs insulation dispersion 30min again with stirring velocity, obtain carboxylic acid type cellulose acetate emulsion,
The ratio of cellulose acetate, triethylamine and deionized water that the Diisopropyl azodicarboxylate of described vinylformic acid, Hydroxyethyl acrylate, butanone, recrystallization, dibutyl tin laurate, isophorone diisocyanate, methyl acetate dissolve is 2g:2g:15g:0.3g:0.2g:3g:2g:3g:60ml.
Embodiment five
The preparation method of carboxylic acid type cellulose acetate emulsion of the present invention comprises the following steps:
Take vinylformic acid, Hydroxyethyl acrylate, the Diisopropyl azodicarboxylate of butanone and recrystallization, again by vinylformic acid, Hydroxyethyl acrylate and butanone join in flask, then the Diisopropyl azodicarboxylate of recrystallization is added, constant temperature under the condition of 77 DEG C be 200rpm stirring reaction 1.5h with speed, the dibutyl tin laurate after the process of 4A molecular sieve dehydration and isophorone diisocyanate is added after being cooled to 50 DEG C, and carry out constant temperature stirring reaction 1h, wherein, stirring velocity is 400rpm, be warming up to 65 DEG C again, then the cellulose acetate that methyl acetate dissolves is added, 50 DEG C are cooled to after insulation reaction 2h, add triethylamine again, 35 DEG C are cooled to after insulation salify, then deionized water is added, be that 2000rpm stirs insulation dispersion 30min again with stirring velocity, obtain carboxylic acid type cellulose acetate emulsion,
The ratio of cellulose acetate, triethylamine and deionized water that the Diisopropyl azodicarboxylate of described vinylformic acid, Hydroxyethyl acrylate, butanone, recrystallization, dibutyl tin laurate, isophorone diisocyanate, methyl acetate dissolve is 7g:5g:25g:8g:7g:7g:5g:8g:60ml.
Embodiment six
The preparation method of carboxylic acid type cellulose acetate emulsion of the present invention comprises the following steps:
Take vinylformic acid, Hydroxyethyl acrylate, the Diisopropyl azodicarboxylate of butanone and recrystallization, again by vinylformic acid, Hydroxyethyl acrylate and butanone join in flask, then the Diisopropyl azodicarboxylate of recrystallization is added, constant temperature under the condition of 74 DEG C be 200rpm stirring reaction 1.5h with speed, the dibutyl tin laurate after the process of 4A molecular sieve dehydration and isophorone diisocyanate is added after being cooled to 48 DEG C, and carry out constant temperature stirring reaction 1h, wherein, stirring velocity is 400rpm, be warming up to 58 DEG C again, then the cellulose acetate that methyl acetate dissolves is added, 47 DEG C are cooled to after insulation reaction 2h, add triethylamine again, 28 DEG C are cooled to after insulation salify, then deionized water is added, be that 2000rpm stirs insulation dispersion 30min again with stirring velocity, obtain carboxylic acid type cellulose acetate emulsion,
The ratio of cellulose acetate, triethylamine and deionized water that the Diisopropyl azodicarboxylate of described vinylformic acid, Hydroxyethyl acrylate, butanone, recrystallization, dibutyl tin laurate, isophorone diisocyanate, methyl acetate dissolve is 6g:5.5g:16g:0.8g:0.3g:6.5g:5.5g:5.5g:60ml.
When the carboxylic acid type cellulose acetate emulsion prepared by the present invention prepares glued membrane, only need pour carboxylic acid type cellulose acetate emulsion in polyfluortetraethylene plate casting film-forming, ambient temperatare puts 24h, put into drying oven again to take out after dry 24h at 40 DEG C, after cooling, obtain glued membrane, wherein the thickness 1mm of glued membrane.
The median size d of carboxylic acid type cellulose acetate emulsion prepared by the present invention
n=70nm ~ 200nm size distribution PDI=0.085 ~ 0.120; Carboxylic acid type cellulose acetate emulsion appearance: oyster white (transparent), blueing light, without precipitation; Tensile strength=the 18.5MPa of glued membrane, elongation at break=331.8%.
Claims (7)
1. a preparation method for carboxylic acid type cellulose acetate emulsion, is characterized in that, comprises the following steps:
Take vinylformic acid, Hydroxyethyl acrylate, the Diisopropyl azodicarboxylate of butanone and recrystallization, again by vinylformic acid, Hydroxyethyl acrylate and butanone join in flask, then the Diisopropyl azodicarboxylate of recrystallization is added, constant temperature stirring reaction under the condition of 70-78 DEG C, dibutyl tin laurate and isophorone diisocyanate is added after being cooled to 40-55 DEG C, and carry out constant temperature stirring reaction, be warming up to 50-70 DEG C again, then the cellulose acetate that methyl acetate dissolves is added, 35-55 DEG C is cooled to after insulation reaction, add triethylamine again, 20-40 DEG C is cooled to after insulation salify, then deionized water is added, carry out stirring insulation dispersion again, obtain carboxylic acid type cellulose acetate emulsion.
2. the preparation method of carboxylic acid type cellulose acetate emulsion according to claim 1, it is characterized in that, the ratio of cellulose acetate, triethylamine and deionized water that the Diisopropyl azodicarboxylate of described vinylformic acid, Hydroxyethyl acrylate, butanone, recrystallization, dibutyl tin laurate, isophorone diisocyanate, methyl acetate dissolve is 1.0-8g:0.5-6.0g:10-30g:0.1-1g:0.1-0.8g:1.0-8.0g:1.0-6.0g: 1.0-9.0g:60ml.
3. the preparation method of carboxylic acid type cellulose acetate emulsion according to claim 1, is characterized in that, under the condition of 70-78 DEG C constant temperature stirring reaction process in the speed that stirs be 200rpm, the reaction times is 1.5h.
4. the preparation method of carboxylic acid type cellulose acetate emulsion according to claim 1, is characterized in that, adds the dibutyl tin laurate after the process of 4A molecular sieve dehydration and isophorone diisocyanate after being cooled to 40-55 DEG C.
5. the preparation method of carboxylic acid type cellulose acetate emulsion according to claim 1, it is characterized in that, after being cooled to 40-55 DEG C, add dibutyl tin laurate and isophorone diisocyanate, and constant temperature stirring reaction 1h, wherein, the speed of stirring is 400rpm.
6. the preparation method of carboxylic acid type cellulose acetate emulsion according to claim 1, is characterized in that, be cooled to 35-55 DEG C after insulation reaction 2h.
7. the preparation method of carboxylic acid type cellulose acetate emulsion according to claim 1, is characterized in that, stirring the speed stirred in the process of insulation dispersion is 2000rpm, and the time of insulated and stirred dispersion is 30min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510872908.6A CN105440251A (en) | 2015-12-01 | 2015-12-01 | Preparation method of carboxylate acetate fiber emulsion |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510872908.6A CN105440251A (en) | 2015-12-01 | 2015-12-01 | Preparation method of carboxylate acetate fiber emulsion |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105440251A true CN105440251A (en) | 2016-03-30 |
Family
ID=55550925
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510872908.6A Pending CN105440251A (en) | 2015-12-01 | 2015-12-01 | Preparation method of carboxylate acetate fiber emulsion |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105440251A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107057025A (en) * | 2017-01-22 | 2017-08-18 | 陕西科技大学 | A kind of preparation method of environmental-friendly aqueous acetate fiber emulsion |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101437484A (en) * | 2006-04-07 | 2009-05-20 | 拜尔材料科学股份公司 | Nitrocellulose-based binders for aqueous nail polishes |
| CN101486798A (en) * | 2009-02-13 | 2009-07-22 | 西安交通大学 | Self-emulsifying aqueous nitrocellulose emulsion and preparation thereof |
| CN104479137A (en) * | 2014-12-03 | 2015-04-01 | 陕西科技大学 | Preparation method of water-based nitrocellulose emulsion and nitrocellulose film |
-
2015
- 2015-12-01 CN CN201510872908.6A patent/CN105440251A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101437484A (en) * | 2006-04-07 | 2009-05-20 | 拜尔材料科学股份公司 | Nitrocellulose-based binders for aqueous nail polishes |
| CN101486798A (en) * | 2009-02-13 | 2009-07-22 | 西安交通大学 | Self-emulsifying aqueous nitrocellulose emulsion and preparation thereof |
| CN104479137A (en) * | 2014-12-03 | 2015-04-01 | 陕西科技大学 | Preparation method of water-based nitrocellulose emulsion and nitrocellulose film |
Non-Patent Citations (1)
| Title |
|---|
| 黄玉媛等: "《精细化工配方研究与产品配制技术》", 30 June 2003 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107057025A (en) * | 2017-01-22 | 2017-08-18 | 陕西科技大学 | A kind of preparation method of environmental-friendly aqueous acetate fiber emulsion |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101457005B (en) | Method for preparing hydroxyl acrylic acid water dispersoid | |
| CN104479137B (en) | Preparation method of water-based nitrocellulose emulsion and nitrocellulose film | |
| CN103937428B (en) | A kind of preparation method of modified corn starch sizing agent | |
| US20090018252A1 (en) | Aqueous emulsion and coating | |
| CN103131354B (en) | Styrene modified polyvinyl acetate emulsion and preparation method | |
| CN104231188B (en) | A kind of esters polycarboxylic acid slump retaining agent and preparation method thereof | |
| CN107057025A (en) | A kind of preparation method of environmental-friendly aqueous acetate fiber emulsion | |
| CN104109220A (en) | Composite modified starch emulsion for coating and preparation method of emulsion | |
| CN103951789B (en) | A kind of resistant to elevated temperatures minute surface silver resin and preparation method thereof | |
| CN103739769A (en) | Method for preparing novel hydrophobic association type polymer surfactant | |
| CN105440236A (en) | Preparation method of sulfonate type water-borne cellulose acetate emulsion | |
| CN107653704B (en) | Fiber stock solution color paste and preparation method thereof | |
| CN105440251A (en) | Preparation method of carboxylate acetate fiber emulsion | |
| CN104974307B (en) | Inorganic silicon maleic anhydride grafted polyethylene alcohol material and preparation method and application | |
| CN105199049A (en) | Hydroxyl acrylic emulsion of core-shell structure and preparing method thereof | |
| CN107903367A (en) | A kind of preparation method and product of self-emulsifying aqueous acetate fiber lotion | |
| CN101096393B (en) | Macromolecule dispersant for inorganic pigment and filler and preparation method thereof | |
| CN100572406C (en) | A kind of hydrophobicity redispersable latex powder | |
| CN105349039A (en) | Colorized wear-resisting raw lacquer coating and preparation method thereof | |
| CN103820061A (en) | Adhesive for plastic-wood composite materials and preparation method thereof | |
| CN103923262A (en) | Method for grafting and modifying chlorinated polypropylene through maleic anhydride | |
| CN111253588A (en) | Preparation method of modified mica powder/waterborne acrylate micro-nano composite emulsion | |
| CN107459618B (en) | A kind of preparation method of woodcare paint water-based acrylic resin and the product of acquisition | |
| CN104789030A (en) | Film-forming assistant for environment-friendly latex paints and preparation method thereof | |
| CN105440235A (en) | Preparation method of sulfonate type water-borne nitrocellulose emulsion |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20160330 |
|
| RJ01 | Rejection of invention patent application after publication |