CN110016808A - A kind of preparation method of graft starch composite gelatin albumen slurry - Google Patents
A kind of preparation method of graft starch composite gelatin albumen slurry Download PDFInfo
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- CN110016808A CN110016808A CN201910151060.6A CN201910151060A CN110016808A CN 110016808 A CN110016808 A CN 110016808A CN 201910151060 A CN201910151060 A CN 201910151060A CN 110016808 A CN110016808 A CN 110016808A
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- D06M13/224—Esters of carboxylic acids; Esters of carbonic acid
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- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/01—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
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- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
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- D06M15/03—Polysaccharides or derivatives thereof
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- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/327—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated alcohols or esters thereof
- D06M15/333—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated alcohols or esters thereof of vinyl acetate; Polyvinylalcohol
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- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/40—Reduced friction resistance, lubricant properties; Sizing compositions
Abstract
The present invention relates to a kind of preparation methods of graft starch composite gelatin albumen slurry, belong to textile material technical field.The present invention passes through addition hydrogenation sheep oil and rilanit special, prepare composite mortar, hydrogenate sheep oil and rilanit special has emulsibility under the action of tridecanol polyoxyethylene ether and monoglyceride, it can be equably miscible in slurries, play plasticization, improve the rate of sizing of slurry, when grease is added in the adhesive agent of polar functionalities, grease molecules can destroy the physical crosslinking point of adhesive agent macromolecular, so that interaction and hydrogen bond cannot be established between macromolecular polar group, original segment that can not be moved also setting in motion, so the glass transition temperature of serous coat reduces, become more soft, on the other hand, interval between grease molecules reduces the intermolecular cohesiveness of adhesive agent, to serous coat structural relaxation, strength reduction, equally because of the isolation of grease molecules, it hinders and sticks together agent molecule and be sufficiently close together to fiber, slurry can be effectively improved The desizing rate of material.
Description
Technical field
The present invention relates to a kind of preparation methods of graft starch composite gelatin albumen slurry, belong to textile material technology neck
Domain.
Background technique
Spinning sizing agent is divided into adhesive agent and sizing auxiliary agent two major classes, and adhesive agent is the primary raw material for forming slurries, determines
The sizing performance of slurries, and sizing auxiliary agent can improve the defect or deficiency of the certain performances of adhesive agent.Grease, also known as wax disk(-sc),
It is a most commonly used analog assistant in sizing auxiliary agent.Yam surface friction factor can be effectively reduced with grease using sizing, subtract
End breakage when weaving less improves weaving efficiency.Grease is also referred to as higher fatty acid ester, is a kind of complicated
Mixture, it is the general name of oil & fat.Glyceride containing a large amount of unsaturated fatty acids is a kind of liquid at room temperature
Oil；Glyceride containing saturated fatty acid is a kind of solid rouge at room temperature.Grease used in sizing be by emulsification or its
He is handled chemical method, so that grease has emulsibility, it can be equably miscible in slurries.In grease addition slurries, oil
Rouge molecule is just diffused into adhesive agent.Due to the addition of grease molecules, the interval between adhesive agent macromolecular chain is widened, greatly
Intermolecular force between molecule segment is weakened, and the interior frictional resistance moved each other between segment reduces, so play plasticising
Effect.When grease is added in the adhesive agent of polar functionalities, grease molecules can destroy the physical crosslinking of adhesive agent macromolecular
Point can not form crosslinking points so that cannot establish interaction and hydrogen bond between macromolecular polar group, original to move
Segment also setting in motion become more soft so the glass transition temperature of serous coat reduces.On the other hand, between grease molecules
Interval reduces the intermolecular cohesiveness of adhesive agent, thus serous coat structural relaxation, strength reduction.Equally because grease molecules every
From hindering and stick together agent molecule and be sufficiently close together to fiber, affect the binding force for sticking together agent molecule Yu fiber macromolecular, stick strong
Degree decline.
Sizing auxiliary agent field is wide, and the shortcoming of main slurry performance is on the one hand filled up in slurries, on the other hand may be used also
To assist main slurry performance preferably to play, to improve sizing quality.The quality of auxiliary agent directly affects the effect of sizing.Now
Spinning sizing agent enterprise is many, and product quality is multifarious, therefore prudent to the selection of auxiliary agent.
Sizing auxiliary agent used at present includes soft lubricant (grease type, wax class), emulsifier, hygroscopic agent, bleeding agent, increasing
Agent, antistatic agent, after waxing, defoaming agent etc. are moulded, most of auxiliary agent influences less or influences very little on serum viscosity, partially helps
Agent can be such that the viscosity of slurries increases, and the phenomenon that gel and adhesive force decline occur.Serum viscosity is that one of sizing technique is important
Parameter, in sizing process, it is desirable that slurries have viscosity appropriate and stability of viscidity is good, because viscosity directly affects the rate of sizing and upper
Starch quality.The reason of leading to slurries increasing stick, has very much, and domestic some researchs think that the use with polyacrylic size has more
It closes, but can also find the addition of some sizing greases so that the phenomenon that slurries thicken in production, it is considered that with grease
It is related that middle natural oil or stearate moiety are saponified the fatty acid salt to be formed.Also the finish of certain fat-free hydrochlorates is documented
Farinaceous size increasing stick is also resulted in, this has certain close because of but rarely found report with emulsifier contained in finish.
To stablize the slurries that grease is added, emulsifier plays a crucial role.Emulsifier alkyl phenol polyoxyethylene ether (APEO)
Chemical property is stablized, as soaking, be impregnated with, emulsify and the primary raw material of cleaning function auxiliary agent, Zeng Yidu are widely used
In textile printing and dyeing processing, but finally because it is not environmentally disabled.The disabling of APEO causes pavilion in textile printing and dyeing industry immediately
Right big wave.Therefore it is badly in need of finding a kind of environment-friendly type emulsifier to replace APEO, this is also the research emphasis of this project.It was weaving
Cheng Zhong, warp thread will not only bear the friction repeatedly from menopause tablet, reed and heald etc., still suffer from the play between yarn
Strong friction then improves the flatness of sizing and reduces the free-revving engine that friction factor is yarn sizing.So in slurries in addition to
Contain adhesive agent, it is also necessary to suitable addition soft lubricant.This is because the plasticity of serous coat can be improved in soft lubricant,
Film rigidity is reduced, film forming is soft, and the flat lubricant nature of sizing is improved, the friction factor of yam surface is reduced, thus when reducing weaving
Warp end break, Lai Tigao loom efficiency.Soft lubricant generally all contains surfactant, can promote wetting of the slurries to warp thread
And penetrating power.Some soft lubricants also contain antistatic agent and fungusproof anti-corrosion agent, can assign sizing antistatic property and mould proof
Anti-corrosive properties.
Domestic sizing wax disk(-sc) is divided into two classes at present, and one kind is petroleum type wax disk(-sc), generally using 58 DEG C of full oil refining rouge as raw material
Solid fraction or liquid wax disk(-sc) are made together with other additives.Paraffin is higher aliphatic paraffins mixture, is insoluble in water, to soda acid
Etc. chemical substances it is highly stable, with slurries formed be incompatible body because, affect serum viscosity stability and adhesive force,
It is unfavorable for the breaking strength of serous coat, is not easy desizing, wax spot occurs after causing dyeing and printing process, seriously affected textile processing matter
Amount；Another kind of is compound non-petroleum type grease, domestic generally by adding partly-hydrolysed animal oil, this product effectively at
Divide 35% or so, but is not especially considerable to the effect for improving sizing flatness.The CD-52 of external such as U.S. Xi Da company
Wax disk(-sc), AVEBE company, Holland SOLWAXC50 be solid wax disk(-sc), flatness is good, the final finishing of fabric will not be influenced, but
It is on the high side.Despite this, textile mills' majority is ready also not liking using the higher non-petroleum type grease of price using price
Lower petroleum type wax disk(-sc).It in view of product quality and increases economic efficiency, textile enterprise is unexpectedly mutually in high-grade fabric articles using non-
Petroleum wax pattern grease auxiliary agent, especially outlet fabric.However non-petroleum weaving grease auxiliary agent also has certain disadvantage, such as production item
Part is harsh, needs hot environment, some the problems such as there is also waste and pollutions.
The wax disk(-sc) that tradition uses is mostly hydro carbons organic compound, and property is stablized, and forms incompatible body because affecting with slurries
The strength of serous coat and Adhesion property to yarn, and desizing is difficult, influences printing quality.Novel sizing is using hydrogenation with grease
Animal and vegetable oil and emulsifier are made, presently, there are the problem of, first is that emulsifier is not environmentally；Second is that environment-friendly type emulsifier makes slurries
Increasing stick influences being normally carried out for slashing technique.Serum viscosity is an important parameter in sizing process, it requires serum viscosity
Appropriate and stability of viscidity is good, and the sizing for then studying a kind of not increasing stick is particularly important with grease.
Summary of the invention
The technical problems to be solved by the invention: incompatible body is formed because influencing serous coat for traditional wax disk(-sc) and slurries
Strength and to the Adhesion property of yarn, desizing is difficult, and not environmentally, environment-friendly type emulsifier makes slurries increasing stick to conventional emulsifier, influences
The problem of being normally carried out of slashing technique provides a kind of preparation method of graft starch composite gelatin albumen slurry.
In order to solve the above technical problems, the technical solution adopted by the present invention is that:
(1) gelatin is added in 3/4 deionized water, with the stirring of 150 ~ 200r/min revolving speed under 60 ~ 70 DEG C of water bath condition
40 ~ 60min obtains glutin solution；
(2) tridecanol polyoxyethylene ether, monoglyceride are added in remaining 1/4 deionized water, under 60 ~ 70 DEG C of water bath condition
10 ~ 20min is stirred with 600 ~ 800r/min revolving speed, obtains emulsifier solution；
(3) part is hydrogenated into sheep oil, rilanit special is added in emulsifier solution, under 75 ~ 85 DEG C of water bath condition with 400 ~
500r/min stirs 10 ~ 20min, obtains pre-emulsion；
(4) polymaleic anhydride graft starch, polyvinyl alcohol are added in glutin solution, under 70 ~ 80 DEG C of water bath condition
20 ~ 30min is stirred with 200 ~ 300r/min revolving speed, heat preservation obtains mixed solution；
(5) pre-emulsion is slowly added dropwise into mixed solution, and ammonium persulfate is added, under 70 ~ 80 DEG C of water bath condition with
300 ~ 340r/min revolving speed constant temperature stirs 2 ~ 4h, obtains mixed reaction solution；
(6) pH to 7 for adjusting mixed reaction solution, is cooled to room temperature, obtains graft starch composite gelatin albumen slurry.
The gelatin, polymaleic anhydride graft starch, hydrogenation sheep oil, rilanit special, polyvinyl alcohol, tridecanol polyoxy
Vinethene, monoglyceride, ammonium persulfate, deionized water parts by weight be that 10 ~ 20 parts of gelatin, the grafting of 20 ~ 40 parts of polymaleic anhydride are formed sediment
Powder, 4 ~ 8 parts of hydrogenation sheep oils, 4 ~ 8 parts of rilanit specials, 5 ~ 10 parts of polyvinyl alcohol, 1 ~ 3 part of tridecanol polyoxyethylene ether, 2 ~ 4 parts of lists
Sweet ester, 0.1 ~ 0.3 part of ammonium persulfate, 80 ~ 100 parts of deionized waters.
The dropwise addition rate of pre-emulsion described in step (5) is 10 ~ 20mL/min.
PH described in step (6) adjusts the ammonium hydroxide using mass concentration 1%.
The specific preparation step of polymaleic anhydride graft starch described in step (4) are as follows:
(1) purified starch is added in deionized water, 20 ~ 30min is stirred with 120 ~ 160r/min revolving speed under room temperature, shallow lake must be refined
Powder dispersion liquid；
(2) purified starch dispersion liquid is placed under 30 ~ 40 DEG C of water-bath, adjusts pH to 3 ~ 4, is passed through nitrogen protection, obtains reactant
System；
(3) hydrogenperoxide steam generator, ferric sulfate, ammonium sulfate are added in reaction system, and will with the rate of addition of 10 ~ 20mL/min
Polymaleic anhydride is slowly added dropwise to reaction system, in the nitrogen atmosphere of 20 ~ 30mL/min flow velocity, 30 ~ 40 DEG C of water-bath item
30 ~ 40min is stirred with 200 ~ 300r/min revolving speed under part, obtains reaction solution；
(4) reaction solution pH to 6 ~ 7 is adjusted, vacuum filtration takes filter cake ethanol solution and deionized water to wash respectively 3 ~ 5 times, sets
Dry 1 ~ 2h, ground 80 ~ 100 mesh obtain polymaleic anhydride graft starch under conditions of 40 ~ 50 DEG C in baking oven.
The exquisite cornstarch, polymaleic anhydride, deionized water, hydrogenperoxide steam generator, ferric sulfate, ammonium sulfate weight
Measuring part is 60 ~ 80 parts of exquisite cornstarch, 6 ~ 8 parts of polymaleic anhydride, 120 ~ 180 parts of deionized waters, 15 ~ 20 parts of mass concentrations 1%
Hydrogenperoxide steam generator, 0.2 ~ 0.4 part of ferric sulfate, 0.3 ~ 0.5 part of ammonium sulfate.
Nitrogen flow rate described in step (2) is 20 ~ 30mL/min, adjusts pH using the hydrochloric acid of mass concentration 1%.
PH is adjusted described in step (4) using the sodium carbonate liquor of mass concentration 1%.
The specific preparation step of purified starch described in step (1) are as follows:
(1) methanol is added in deionized water, 10 ~ 15min is stirred with 200 ~ 240r/min revolving speed under room temperature, obtains methanol solution；
(2) cornstarch is added in methanol solution, 20 ~ 30min is stirred with 100 ~ 120r/min revolving speed under room temperature, obtain starch point
Dispersion liquid；
(3) starch dispersion liquid is placed under 50 ~ 60 DEG C of water bath condition and 1 ~ 2h is stirred in the twinkling of an eye with 120 ~ 140r/min, vacuum is taken out
Filter, filter cake are placed at 60 ~ 80 DEG C dry 1 ~ 2h, 80 ~ 100 meshes are crossed after grinding, obtain purified starch,
The cornstarch, methanol, deionized water parts by weight be 60 ~ 80 parts of cornstarch, 120 ~ 150 parts of methanol, 15 ~ 20
Part deionized water.
The present invention is compared with other methods, and advantageous effects are:
(1) present invention prepares composite mortar using polymaleic anhydride graft starch and gelatin as raw material, and starch is a kind of reproducible
Natural polymer has the advantages that source is wide, biodegradable, has many polar hydroxyls in starch polymer, it
Between hydrogen bond easy to form, therefore to the strong fiber of polarity have good adhesion strength, the obvolvent between single fiber can be enhanced
Power improves yarn strength, and docile yam surface filoplume, and the amylose molecule chain of line style is easily arranged in parallel, passes through hydroxyl
Between hydrogen bond formed association, when farinaceous size is denseer, amylose gel easy to form, have preferable film forming, and
Serous coat has the physical mechanical properties such as good breaking strength, elongation at break, wearability, the hydroxyl on starch polymer and poly- horse
Carry out acid anhydrides to react, form cross-linking system, improve the viscosity, stability and heat resistance of starch, improves the rate of sizing, poly- horse
Carrying out acid anhydrides can be effectively reduced the activation energy of glucoside key in starch polymer, and the hydrolysis of catalytic starch reduces the degree of polymerization of starch, makes
The viscosity for obtaining farinaceous size reduces, and improves the mobility of slurries, to keep slurry sizing uniform, desizing is easy, and glutin is
A kind of natural macromolecular substance can form viscosity colloid in water, have good adhesiveness to natural fiber, and have good
Good filming performance, the gelatin film wearability of formation is good, facile hydrolysis can be made by the way that glutin and graft starch is compound
Gelatin while retaining original advantageous property again with grafted protein is compound obtains good mechanics ability, to overcome its brittleness
Big disadvantage improves the mechanical strength and adhesiveness of serous coat, improves the desizability of slurry；
(2) present invention prepares composite mortar by addition hydrogenation sheep oil and rilanit special, hydrogenates sheep oil and rilanit special exists
There is emulsibility under the action of tridecanol polyoxyethylene ether and monoglyceride, can be equably miscible in slurries, when grease is added
In slurries, grease molecules are just diffused into adhesive agent, due to the addition of grease molecules, have been widened between adhesive agent macromolecular chain
Interval, the intermolecular force between macromolecular chain segment is weakened, and the interior frictional resistance moved each other between segment reduces, so
Plasticization is played, the rate of sizing of slurry is improved, when grease is added in the adhesive agent of polar functionalities, grease molecules can be broken
The physical crosslinking point of bad adhesive agent macromolecular, so that interaction and hydrogen bond cannot be established between macromolecular polar group, it can not
Crosslinking points are formed, also setting in motion so the glass transition temperature of serous coat reduces becomes more soft to original segment that can not be moved
Soft, on the other hand, the interval between grease molecules reduces the intermolecular cohesiveness of adhesive agent, thus serous coat structural relaxation, intensity
It reduces, equally because of the isolation of grease molecules, hinders and stick together agent molecule and be sufficiently close together to fiber, affect and stick together agent molecule and fine
Tie up the binding force of macromolecular, adhesion strength decline, so as to effectively improve the desizing rate of slurry.
Specific embodiment
According to parts by weight, 60 ~ 80 parts of cornstarch, 120 ~ 150 parts of methanol, 15 ~ 20 parts of deionized waters are weighed respectively, it will
Methanol is added in deionized water, stirs 10 ~ 15min under room temperature with 200 ~ 240r/min revolving speed, methanol solution is obtained, by cornstarch
It is added in methanol solution, 20 ~ 30min is stirred with 100 ~ 120r/min revolving speed under room temperature, starch dispersion liquid is obtained, by starch dispersion liquid
It is placed under 50 ~ 60 DEG C of water bath condition and 1 ~ 2h is stirred in the twinkling of an eye with 120 ~ 140r/min, be filtered by vacuum, filter cake is placed in 60 ~ 80 DEG C
1 ~ 2h of lower drying crosses 80 ~ 100 meshes, obtains purified starch, then according to parts by weight after grinding, weigh 60 ~ 80 parts of exquisite jade respectively
Rice starch, 6 ~ 8 parts of polymaleic anhydride, 120 ~ 180 parts of deionized waters, the hydrogenperoxide steam generator of 15 ~ 20 parts of mass concentrations 1%, 0.2 ~
0.4 part of ferric sulfate, 0.3 ~ 0.5 part of ammonium sulfate purified starch are added in deionized water, with 120 ~ 160r/min revolving speed under room temperature
20 ~ 30min is stirred, purified starch dispersion liquid is obtained, purified starch dispersion liquid is placed under 30 ~ 40 DEG C of water-bath, it is dense that quality is added dropwise
The salt acid for adjusting pH of degree 1% is passed through nitrogen protection with the air velocity of 20 ~ 30mL/min, obtains reaction system, by peroxidating to 3 ~ 4
Hydrogen solution, ferric sulfate, ammonium sulfate are added in reaction system, and with the rate of addition of 10 ~ 20mL/min that polymaleic anhydride is slow
Be added dropwise in system, in the nitrogen atmosphere of 20 ~ 30mL/min flow velocity, under 30 ~ 40 DEG C of water bath condition with 200 ~ 300r/min
Revolving speed stirs 30 ~ 40min, obtains reaction solution, and the sodium carbonate liquor that mass concentration 1% is added dropwise into reaction solution adjusts pH to 6 ~ 7, very
Empty pump filter, takes filter cake ethanol solution and deionized water to wash respectively 3 ~ 5 times, is placed in baking oven and does under conditions of 40 ~ 50 DEG C
Dry 1 ~ 2h, ground 80 ~ 100 mesh, obtains polymaleic anhydride graft starch, then according to parts by weight, and 10 ~ 20 parts of weighing is bright respectively
Glue, 20 ~ 40 parts of polymaleic anhydride graft starch, 4 ~ 8 parts of hydrogenation sheep oils, 4 ~ 8 parts of rilanit specials, 5 ~ 10 parts of polyvinyl alcohol, 1 ~ 3
Part tridecanol polyoxyethylene ether, 2 ~ 4 parts of monoglycerides, 0.1 ~ 0.3 part of ammonium persulfate, 80 ~ 100 parts of deionized waters, gelatin is added
In 3/4 deionized water, 40 ~ 60min is stirred with 150 ~ 200r/min revolving speed under 60 ~ 70 DEG C of water bath condition, obtains gelatin egg
White solution tridecanol polyoxyethylene ether, monoglyceride is added in remaining 1/4 deionized water, under 60 ~ 70 DEG C of water bath condition
10 ~ 20min is stirred with 600 ~ 800r/min revolving speed, obtains emulsifier solution, part is hydrogenated into sheep oil, emulsifier is added in rilanit special
In solution, 10 ~ 20min is stirred with 400 ~ 500r/min under 75 ~ 85 DEG C of water bath condition, pre-emulsion is obtained, by poly
Acid anhydride graft starch, polyvinyl alcohol are added in glutin solution, with 200 ~ 300r/min revolving speed under 70 ~ 80 DEG C of water bath condition
20 ~ 30min is stirred, heat preservation obtains mixed solution, pre-emulsion is slowly added dropwise with the flow velocity of 10 ~ 20mL/min to mixed solution
In, and ammonium persulfate is added, 2 ~ 4h is stirred with 300 ~ 340r/min revolving speed constant temperature under 70 ~ 80 DEG C of water bath condition, must be mixed
Reaction solution, the ammonium hydroxide that mass concentration 1% is added dropwise into mixed reaction solution adjust pH to 7, are cooled to room temperature, it is compound to obtain graft starch
Glutin slurry.
Embodiment 1
According to parts by weight, 60 parts of cornstarch, 120 parts of methanol, 15 parts of deionized waters are weighed respectively, and deionization is added in methanol
In water, 10min is stirred with 200r/min revolving speed under room temperature, obtains methanol solution, cornstarch is added in methanol solution, under room temperature
20min is stirred with 100r/min revolving speed, starch dispersion liquid is obtained, starch dispersion liquid is placed under 50 DEG C of water bath condition with 120r/
Min stirs 1h in the twinkling of an eye, vacuum filtration, and filter cake is placed at 60 DEG C dry 1h, and 80 meshes are crossed after grinding, obtain purified starch, then press
Parts by weight meter weighs 60 parts of exquisite cornstarch, 6 parts of polymaleic anhydride, 120 parts of deionized waters, 15 parts of mass concentrations respectively
1% hydrogenperoxide steam generator, 0.2 part of ferric sulfate, 0.3 part of ammonium sulfate, by purified starch be added deionized water in, under room temperature with
120r/min revolving speed stirs 20min, obtains purified starch dispersion liquid, purified starch dispersion liquid is placed under 30 DEG C of water-bath, is added dropwise
The salt acid for adjusting pH of mass concentration 1% is passed through nitrogen protection to 3, with the air velocity of 20mL/min, obtains reaction system, by peroxide
Change hydrogen solution, ferric sulfate, ammonium sulfate to be added in reaction system, and slowly drip polymaleic anhydride with the rate of addition of 10mL/min
It adds in system, is stirred in the nitrogen atmosphere of 20mL/min flow velocity, under 30 DEG C of water bath condition with 200r/min revolving speed
30min obtains reaction solution, and the sodium carbonate liquor that mass concentration 1% is added dropwise into reaction solution adjusts pH to 6, and vacuum filtration takes filter cake
It is washed respectively 3 times with ethanol solution and deionized water, is placed in baking oven and dries 1h under conditions of 40 DEG C, ground 80 mesh,
Polymaleic anhydride graft starch is obtained, then according to parts by weight, weighs 10 parts of gelatin, 20 parts of polymaleic anhydride graft starch, 4 respectively
Part hydrogenation sheep oil, 4 parts of rilanit specials, 5 parts of polyvinyl alcohol, 1 part of tridecanol polyoxyethylene ether, 2 parts of monoglycerides, 0.1 part of over cure
Sour ammonium, 80 parts of deionized waters gelatin are added in 3/4 deionized water, with 150r/min revolving speed under 60 DEG C of water bath condition
40min is stirred, glutin solution is obtained, tridecanol polyoxyethylene ether, monoglyceride are added in remaining 1/4 deionized water,
10min is stirred with 600r/min revolving speed under 60 DEG C of water bath condition, obtains emulsifier solution, part is hydrogenated into sheep oil, rilanit special
It is added in emulsifier solution, 10min is stirred with 400r/min under 75 DEG C of water bath condition, pre-emulsion is obtained, by poly
Acid anhydride graft starch, polyvinyl alcohol are added in glutin solution, with the stirring of 200r/min revolving speed under 70 DEG C of water bath condition
20min, heat preservation, obtains mixed solution, pre-emulsion is slowly added dropwise with the flow velocity of 10mL/min into mixed solution, and was added
Ammonium sulfate stirs 2h under 70 DEG C of water bath condition with 300r/min revolving speed constant temperature, mixed reaction solution is obtained, into mixed reaction solution
The ammonium hydroxide that mass concentration 1% is added dropwise adjusts pH to 7, is cooled to room temperature, obtains graft starch composite gelatin albumen slurry.
Embodiment 2
According to parts by weight, 70 parts of cornstarch, 135 parts of methanol, 17 parts of deionized waters are weighed respectively, and deionization is added in methanol
In water, 13min is stirred with 220r/min revolving speed under room temperature, obtains methanol solution, cornstarch is added in methanol solution, under room temperature
25min is stirred with 110r/min revolving speed, starch dispersion liquid is obtained, starch dispersion liquid is placed under 55 DEG C of water bath condition with 130r/
Min stirs 1.5h in the twinkling of an eye, vacuum filtration, and filter cake is placed at 70 DEG C dry 1.5h, and 90 meshes are crossed after grinding, obtain purified starch,
Again according to parts by weight, 70 parts of exquisite cornstarch, 7 parts of polymaleic anhydride, 150 parts of deionized waters, 17 parts of quality are weighed respectively
The hydrogenperoxide steam generator of concentration 1%, 0.3 part of ferric sulfate, 0.4 part of ammonium sulfate purified starch are added in deionized water, under room temperature
25min is stirred with 140r/min revolving speed, purified starch dispersion liquid is obtained, purified starch dispersion liquid is placed under 35 DEG C of water-bath, is dripped
Add the salt acid for adjusting pH of mass concentration 1% to 3.5, nitrogen protection is passed through with the air velocity of 25mL/min, obtains reaction system, it will
Hydrogenperoxide steam generator, ferric sulfate, ammonium sulfate are added in reaction system, and are delayed polymaleic anhydride with the rate of addition of 15mL/min
Slowly it is added dropwise in system, is stirred in the nitrogen atmosphere of 25mL/min flow velocity, under 35 DEG C of water bath condition with 250r/min revolving speed
35min obtains reaction solution, and the sodium carbonate liquor that mass concentration 1% is added dropwise into reaction solution adjusts pH to 6.5, and vacuum filtration takes filter
Cake ethanol solution and deionized water are washed 4 times respectively, are placed in baking oven dry 1.5h, ground 90 mesh under conditions of 45 DEG C
Sieve, obtains polymaleic anhydride graft starch, then according to parts by weight, weighs 15 parts of gelatin respectively, 30 parts of polymaleic anhydride grafting are formed sediment
Powder, 6 parts of hydrogenation sheep oils, 6 parts of rilanit specials, 7 parts of polyvinyl alcohol, 2 parts of tridecanol polyoxyethylene ethers, 3 parts of monoglycerides, 0.2 part
Ammonium persulfate, 90 parts of deionized waters gelatin are added in 3/4 deionized water, with 175r/min under 65 DEG C of water bath condition
Revolving speed stirs 50min, obtains glutin solution, and remaining 1/4 deionized water is added in tridecanol polyoxyethylene ether, monoglyceride
In, 15min is stirred with 700r/min revolving speed under 65 DEG C of water bath condition, obtains emulsifier solution, part is hydrogenated into sheep oil, hydrogenation castor
Sesame oil is added in emulsifier solution, stirs 15min under 80 DEG C of water bath condition with 450r/min, pre-emulsion is obtained, by poly- horse
Maleic anhydride grafted starch, polyvinyl alcohol are added in glutin solution, are stirred under 75 DEG C of water bath condition with 250r/min revolving speed
25min is mixed, is kept the temperature, is obtained mixed solution, pre-emulsion is slowly added dropwise with the flow velocity of 15mL/min into mixed solution, and is added
Ammonium persulfate stirs 3h under 75 DEG C of water bath condition with 320r/min revolving speed constant temperature, mixed reaction solution is obtained, to mixed reaction solution
The middle ammonium hydroxide that mass concentration 1% is added dropwise adjusts pH to 7, is cooled to room temperature, obtains graft starch composite gelatin albumen slurry.
Embodiment 3
According to parts by weight, 80 parts of cornstarch, 150 parts of methanol, 20 parts of deionized waters are weighed respectively, and deionization is added in methanol
In water, 15min is stirred with 240r/min revolving speed under room temperature, obtains methanol solution, cornstarch is added in methanol solution, under room temperature
30min is stirred with 120r/min revolving speed, starch dispersion liquid is obtained, starch dispersion liquid is placed under 60 DEG C of water bath condition with 140r/
Min stirs 2h in the twinkling of an eye, vacuum filtration, and filter cake is placed at 80 DEG C dry 2h, sieves with 100 mesh sieve after grinding, obtains purified starch, then press
Parts by weight meter weighs 80 parts of exquisite cornstarch, 8 parts of polymaleic anhydride, 180 parts of deionized waters, 20 parts of mass concentrations respectively
1% hydrogenperoxide steam generator, 0.4 part of ferric sulfate, 0.5 part of ammonium sulfate, by purified starch be added deionized water in, under room temperature with
160r/min revolving speed stirs 30min, obtains purified starch dispersion liquid, purified starch dispersion liquid is placed under 40 DEG C of water-bath, is added dropwise
The salt acid for adjusting pH of mass concentration 1% is passed through nitrogen protection to 4, with the air velocity of 30mL/min, obtains reaction system, by peroxide
Change hydrogen solution, ferric sulfate, ammonium sulfate to be added in reaction system, and slowly drip polymaleic anhydride with the rate of addition of 20mL/min
It adds in system, is stirred in the nitrogen atmosphere of 30mL/min flow velocity, under 40 DEG C of water bath condition with 300r/min revolving speed
40min obtains reaction solution, and the sodium carbonate liquor that mass concentration 1% is added dropwise into reaction solution adjusts pH to 7, and vacuum filtration takes filter cake
It is washed respectively 5 times with ethanol solution and deionized water, is placed in baking oven dry 2h, grinding under conditions of 50 DEG C and sieves with 100 mesh sieve,
Polymaleic anhydride graft starch is obtained, then according to parts by weight, weighs 20 parts of gelatin, 40 parts of polymaleic anhydride graft starch, 8 respectively
Part hydrogenation sheep oil, 8 parts of rilanit specials, 10 parts of polyvinyl alcohol, 3 parts of tridecanol polyoxyethylene ethers, 4 parts of monoglycerides, 0.3 part of over cure
Sour ammonium, 100 parts of deionized waters gelatin are added in 3/4 deionized water, with 200r/min revolving speed under 70 DEG C of water bath condition
60min is stirred, glutin solution is obtained, tridecanol polyoxyethylene ether, monoglyceride are added in remaining 1/4 deionized water,
20min is stirred with 800r/min revolving speed under 70 DEG C of water bath condition, obtains emulsifier solution, part is hydrogenated into sheep oil, rilanit special
It is added in emulsifier solution, 20min is stirred with 500r/min under 85 DEG C of water bath condition, pre-emulsion is obtained, by poly
Acid anhydride graft starch, polyvinyl alcohol are added in glutin solution, with the stirring of 300r/min revolving speed under 80 DEG C of water bath condition
30min, heat preservation, obtains mixed solution, pre-emulsion is slowly added dropwise with the flow velocity of 20mL/min into mixed solution, and was added
Ammonium sulfate stirs 4h under 80 DEG C of water bath condition with 340r/min revolving speed constant temperature, mixed reaction solution is obtained, into mixed reaction solution
The ammonium hydroxide that mass concentration 1% is added dropwise adjusts pH to 7, is cooled to room temperature, obtains graft starch composite gelatin albumen slurry.
The slurry that graft starch composite gelatin albumen slurry prepared by the present invention and Fujian factory use is detected,
Specific testing result such as following table table 1:
1, the test of the breaking strength of serous coat and elongation at break
The production of serous coat
It is 650mm × 400mm by area, is put on the point of dedicated tripod adjusting screw with a thickness of the polyfluortetraethylene plate of 5mm
On end, is dipped in a small amount of water on polyfluortetraethylene plate, the mylar of 0.3mm thickness is then laid in polyfluortetraethylene plate
On, the slurries of 3% concentration are configured, in 95 DEG C of heat preservation 1h.It is then cooled to which taken amount 400mL at 50 DEG C or so, is slowly poured on poly- four
On vinyl fluoride plate, and gently moved back and forth with glass bar, is paved with slurries on polyfluortetraethylene plate.After spontaneously drying film forming,
Serous coat is peeled from polyfluortetraethylene plate carefully, obtains spare serous coat.
(2) breaking strength of serous coat, elongation at break
Serous coat is cut into 220mm × 5mm bar-shaped sample, constant temperature, humidity room's inner equilibrium are placed on for 24 hours, then in Instron5566 type
Strength aircraft measurements ultimate strength, elongation at break (sample holder distance 100mm, decrease speed 50m/min), every kind of serous coat reality
It tests 30 times, calculates its average value, further according to serous coat THICKNESS CALCULATION breaking strength.
The test of desizing rate:
The desizing rate of 1-3 of the embodiment of the present invention and comparative example, the calculation formula of weight method: (before desizing are tested using weight method
Fabric weight after fabric weight-desizing) fabric weight × 100% before/desizing
1 graft starch composite gelatin albumen slurry performance characterization of table
Graft starch composite gelatin albumen slurry prepared by the present invention as shown in Table 1, mechanical property is good, and desizing rate is high.
Claims (9)
1. a kind of preparation method of graft starch composite gelatin albumen slurry, which is characterized in that specific preparation step are as follows:
(1) gelatin is added in 3/4 deionized water, with the stirring of 150 ~ 200r/min revolving speed under 60 ~ 70 DEG C of water bath condition
40 ~ 60min obtains glutin solution；
(2) tridecanol polyoxyethylene ether, monoglyceride are added in remaining 1/4 deionized water, under 60 ~ 70 DEG C of water bath condition
10 ~ 20min is stirred with 600 ~ 800r/min revolving speed, obtains emulsifier solution；
(3) part is hydrogenated into sheep oil, rilanit special is added in emulsifier solution, under 75 ~ 85 DEG C of water bath condition with 400 ~
500r/min stirs 10 ~ 20min, obtains pre-emulsion；
(4) polymaleic anhydride graft starch, polyvinyl alcohol are added in glutin solution, under 70 ~ 80 DEG C of water bath condition
20 ~ 30min is stirred with 200 ~ 300r/min revolving speed, heat preservation obtains mixed solution；
(5) pre-emulsion is slowly added dropwise into mixed solution, and ammonium persulfate is added, under 70 ~ 80 DEG C of water bath condition with
300 ~ 340r/min revolving speed constant temperature stirs 2 ~ 4h, obtains mixed reaction solution；
(6) pH to 7 for adjusting mixed reaction solution, is cooled to room temperature, obtains graft starch composite gelatin albumen slurry.
2. a kind of preparation method of graft starch composite gelatin albumen slurry according to claim 1, which is characterized in that institute
Gelatin, the polymaleic anhydride graft starch, hydrogenation sheep oil, rilanit special, polyvinyl alcohol, tridecanol polyoxyethylene ether, list stated
Sweet ester, ammonium persulfate, deionized water parts by weight be 10 ~ 20 parts of gelatin, 20 ~ 40 parts of polymaleic anhydride graft starch, 4 ~ 8 parts of hydrogen
Change sheep oil, 4 ~ 8 parts of rilanit specials, 5 ~ 10 parts of polyvinyl alcohol, 1 ~ 3 part of tridecanol polyoxyethylene ether, 2 ~ 4 parts of monoglycerides, 0.1 ~
0.3 part of ammonium persulfate, 80 ~ 100 parts of deionized waters.
3. a kind of preparation method of graft starch composite gelatin albumen slurry according to claim 1, which is characterized in that step
Suddenly the dropwise addition rate of pre-emulsion described in (5) is 10 ~ 20mL/min.
4. a kind of preparation method of graft starch composite gelatin albumen slurry according to claim 1, which is characterized in that step
Suddenly pH described in (6) adjusts the ammonium hydroxide using mass concentration 1%.
5. a kind of preparation method of graft starch composite gelatin albumen slurry according to claim 1, which is characterized in that step
Suddenly the specific preparation step of polymaleic anhydride graft starch described in (4) are as follows:
(1) purified starch is added in deionized water, 20 ~ 30min is stirred with 120 ~ 160r/min revolving speed under room temperature, shallow lake must be refined
Powder dispersion liquid；
(2) purified starch dispersion liquid is placed under 30 ~ 40 DEG C of water-bath, adjusts pH to 3 ~ 4, is passed through nitrogen protection, obtains reactant
System；
(3) hydrogenperoxide steam generator, ferric sulfate, ammonium sulfate are added in reaction system, and will with the rate of addition of 10 ~ 20mL/min
Polymaleic anhydride is slowly added dropwise to reaction system, in the nitrogen atmosphere of 20 ~ 30mL/min flow velocity, 30 ~ 40 DEG C of water-bath item
30 ~ 40min is stirred with 200 ~ 300r/min revolving speed under part, obtains reaction solution；
(4) reaction solution pH to 6 ~ 7 is adjusted, vacuum filtration takes filter cake ethanol solution and deionized water to wash respectively 3 ~ 5 times, sets
Dry 1 ~ 2h, ground 80 ~ 100 mesh obtain polymaleic anhydride graft starch under conditions of 40 ~ 50 DEG C in baking oven.
6. a kind of preparation method of graft starch composite gelatin albumen slurry according to claim 5, which is characterized in that institute
The exquisite cornstarch stated, polymaleic anhydride, deionized water, hydrogenperoxide steam generator, ferric sulfate, ammonium sulfate parts by weight be 60 ~
The peroxidating of 80 parts of exquisite cornstarch, 6 ~ 8 parts of polymaleic anhydride, 120 ~ 180 parts of deionized waters, 15 ~ 20 parts of mass concentrations 1%
Hydrogen solution, 0.2 ~ 0.4 part of ferric sulfate, 0.3 ~ 0.5 part of ammonium sulfate.
7. a kind of preparation method of graft starch composite gelatin albumen slurry according to claim 5, which is characterized in that step
Suddenly nitrogen flow rate described in (2) is 20 ~ 30mL/min, adjusts pH using the hydrochloric acid of mass concentration 1%.
8. a kind of preparation method of graft starch composite gelatin albumen slurry according to claim 5, which is characterized in that step
Suddenly pH is adjusted described in (4) using the sodium carbonate liquor of mass concentration 1%.
9. a kind of preparation method of graft starch composite gelatin albumen slurry according to claim 5, which is characterized in that step
Suddenly the specific preparation step of purified starch described in (1) are as follows:
(1) methanol is added in deionized water, 10 ~ 15min is stirred with 200 ~ 240r/min revolving speed under room temperature, obtains methanol solution；
(2) cornstarch is added in methanol solution, 20 ~ 30min is stirred with 100 ~ 120r/min revolving speed under room temperature, obtain starch point
Dispersion liquid；
(3) starch dispersion liquid is placed under 50 ~ 60 DEG C of water bath condition and 1 ~ 2h is stirred in the twinkling of an eye with 120 ~ 140r/min, vacuum is taken out
Filter, filter cake are placed at 60 ~ 80 DEG C dry 1 ~ 2h, 80 ~ 100 meshes are crossed after grinding, obtain purified starch,
The preparation method of a kind of graft starch composite gelatin albumen slurry according to claim 9, which is characterized in that described
Cornstarch, methanol, deionized water parts by weight be 60 ~ 80 parts of cornstarch, 120 ~ 150 parts of methanol, 15 ~ 20 parts of deionizations
Water.
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