CN109369813A - A kind of dedicated cross-linked esterification oxidation ternary compound modified starch production method of Wall paper adhesive - Google Patents
A kind of dedicated cross-linked esterification oxidation ternary compound modified starch production method of Wall paper adhesive Download PDFInfo
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- CN109369813A CN109369813A CN201811234120.2A CN201811234120A CN109369813A CN 109369813 A CN109369813 A CN 109369813A CN 201811234120 A CN201811234120 A CN 201811234120A CN 109369813 A CN109369813 A CN 109369813A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B31/00—Preparation of derivatives of starch
- C08B31/18—Oxidised starch
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B31/00—Preparation of derivatives of starch
- C08B31/003—Crosslinking of starch
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B31/00—Preparation of derivatives of starch
- C08B31/02—Esters
- C08B31/04—Esters of organic acids, e.g. alkenyl-succinated starch
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J103/00—Adhesives based on starch, amylose or amylopectin or on their derivatives or degradation products
- C09J103/04—Starch derivatives
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J103/00—Adhesives based on starch, amylose or amylopectin or on their derivatives or degradation products
- C09J103/04—Starch derivatives
- C09J103/06—Esters
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J103/00—Adhesives based on starch, amylose or amylopectin or on their derivatives or degradation products
- C09J103/04—Starch derivatives
- C09J103/10—Oxidised starch
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Abstract
A kind of dedicated crosslinking -ester-oxidation ternary compound modified starch production method of Wall paper adhesive, which can be improved the cohesive force and freeze-thaw stability of converted starch, while can use separately as Wall paper adhesive.The present invention is to carry out tri compound reaction of degeneration (RD) processing to starch, prepares the high converted starch of a kind of high anti-freezing, transparency；Using tapioca as raw material, reaction of degeneration (RD) is carried out to starch under the conditions of Different adding amount using crosslinking agent sodium trimetaphosphate (or epoxychloropropane, phosphorus oxychloride), esterifying agent vinylacetate (or acetic anhydride) and oxidizing agent sodium hypochlorite respectively, prepares a kind of composite modified starch；Has the high advantage of high anti-freezing, transparency.
Description
Technical field
The present invention relates to adhesive fields, and in particular to a kind of dedicated cross-linked esterification oxidation tri compound denaturation shallow lake of Wall paper adhesive
Powder producing method.
Background technique
The Wall paper adhesive starch special of prior art production is usually the denaturation way by crosslinking -ester.Product
Frost resistance, transparency are general, and easy gel.Such as esterified and cross-linked starch disclosed in " Jilin agricultural " o. 11th in 2013 prepares work
The research of skill.Product frost resistance, the transparency that denaturation way by being crosslinked -ester obtains are general, are not easy gel.Limit its
The application range of Wall paper adhesive.
Summary of the invention
To solve the above problems, the application provides a kind of dedicated cross-linked esterification oxidation ternary compound modified starch life of Wall paper adhesive
Production method, the preparation method can be improved the cohesive force and freeze-thaw stability of converted starch, while can be separately as Wall paper adhesive
It uses.The present invention is to carry out tri compound reaction of degeneration (RD) processing to starch, prepares the high denaturation of a kind of high anti-freezing, transparency and forms sediment
Powder.
The present invention provides a kind of dedicated cross-linked esterification oxidation ternary compound modified starch production method of Wall paper adhesive, it includes step
It is rapid: using tapioca as raw material, use respectively crosslinking agent sodium trimetaphosphate, epoxychloropropane, in phosphorus oxychloride at least
A kind of, esterifying agent vinylacetate or acetic anhydride and oxidizing agent sodium hypochlorite are denaturalized starch under the conditions of Different adding amount
Reaction, prepares a kind of composite modified starch.
Further, sodium hypochlorite dosage is 10-30g.
Further, the dosage of sodium trimetaphosphate is the 0.01-1g of starch on dry basis quality.
Further, the dosage of vinylacetate is the 5-10g of starch on dry basis quality.
Further, the specific steps of preparation method include:
(1) claim 100g tapioca, be packed into reactor tank, 120g water is added and is dispersed with stirring into uniform starch slurry, will react
Tank moves into the water-bath with blender, stirring, and water-bath is warming up to slurry temperature up to 35-40 DEG C；
(2) 2.5%NaOH is added and adjusts starch slurry to pH10.5-11.5, sodium trimetaphosphate, epoxychloropropane, three is added
At least one of chlorethoxyfos 0.01-1g reacts 1-5 hours；
(3) 10%HCL is added and adjusts starch slurry to pH8.0-9.0, adjusting reaction temperature is 25-30 DEG C, and acetic acid second is added
Enester or acetic anhydride 5-10g, the reaction was continued 1-3 hours；
(4) starch slurry PH7.0-7.5 is adjusted, keeping reaction temperature is 25-30 DEG C, and sodium hypochlorite 10-30g is added, and is continued
React 1-3h；
(5) 10%HCl is added, neutralizes starch slurry, is adjusted to pH5.0-5.2；
(6) it washs, be dehydrated, is dry, out powder.
In a kind of wherein embodiment, water temperature is 36-40 DEG C in heating water bath.
In a kind of wherein embodiment, Wong Kam-po tree extracting solution is added into dextrin after washing, additive amount is every 100g
Add 50mL.
The extracting method of the Wong Kam-po tree extracting solution are as follows: the branches and leaves for crushing Wong Kam-po tree, which are put into ethyl alcohol, to be impregnated 10 days
After be obtained by filtration extracting solution, the weight ratio of Wong Kam-po tree branches and leaves and ethyl alcohol is 1:2.
According to the preparation method of above-described embodiment, using tapioca as raw material, three metaphosphoric acid of crosslinking agent is used respectively
Sodium (or epoxychloropropane, phosphorus oxychloride), esterifying agent vinylacetate (or acetic anhydride) and oxidizing agent sodium hypochlorite add in difference
Reaction of degeneration (RD) is carried out to starch under the conditions of dosage, prepares a kind of composite modified starch；Have high excellent of high anti-freezing, transparency
Point.
Specific embodiment
Below by specific embodiment, invention is further described in detail.
In embodiments of the present invention, a kind of dedicated cross-linked esterification oxidation ternary compound modified starch production of Wall paper adhesive is provided
Method, step include:
(1) claim 100g tapioca, be packed into reactor tank, 120g water is added and is dispersed with stirring into uniform starch slurry, will react
Tank moves into the water-bath with blender, starts to stir, and water-bath is warming up to slurry temperature up to 35-40 DEG C.
(2) addition 2.5%NaOH adjusting starch slurry pH10.5-11.5, addition sodium trimetaphosphate (or epoxychloropropane, three
Chlorethoxyfos) 0.01-1g, reacts 1-5 hours.
(3) 10%HCL is added and adjusts starch slurry pH8.0-9.0, adjusting reaction temperature is 25-30 DEG C, and vinyl acetate is added
Ester (or acetic anhydride) 5-10g, the reaction was continued 1-3 hours.
(4) starch slurry PH7.0-7.5 is adjusted, keeping reaction temperature is 25-30 DEG C, and sodium hypochlorite 10-30g is added, and is continued
React 1-3h.
(5) 10%HCl is added, neutralizes starch slurry, adjusts pH5.0-5.2.
(6) it washs, be dehydrated, is dry, out powder.
Embodiment one
In the present embodiment, the dedicated crosslinking -ester-oxidation ternary compound modified starch production method of Wall paper adhesive is as follows:
(1) claim 100g tapioca, be packed into reactor tank, 120g water is added and is dispersed with stirring into uniform starch slurry, will react
Tank moves into the water-bath with blender, starts to stir, water-bath is warming up to slurry temperature up to 35 DEG C.
(2) 2.5%NaOH is added and adjusts starch slurry pH10.5, sodium trimetaphosphate 0.01g is added, react 1 hour.
(3) 10%HCL is added and adjusts starch slurry pH8.0, adjusting reaction temperature is 25 DEG C, vinylacetate 5g is added, after
Continuous reaction 1 hour.
(4) starch slurry PH7.0 is adjusted, keeping reaction temperature is 25 DEG C, and sodium hypochlorite 10g, the reaction was continued 1h is added.
(5) 10%HCl is added, neutralizes starch slurry, adjusts pH5.0.
(6) it washs, be dehydrated, is dry, out powder.
Embodiment two
In the present embodiment, the dedicated crosslinking -ester-oxidation ternary compound modified starch production method of Wall paper adhesive is as follows:
(1) claim 100g tapioca, be packed into reactor tank, 120g water is added and is dispersed with stirring into uniform starch slurry, will react
Tank moves into the water-bath with blender, starts to stir, water-bath is warming up to slurry temperature up to 40 DEG C.
(2) 2.5%NaOH is added and adjusts starch slurry pH11.5, epoxychloropropane 1g is added, react 5 hours.
(3) 10%HCL is added and adjusts starch slurry pH9.0, adjusting reaction temperature is 30 DEG C, and acetic anhydride 10g is added, and is continued
Reaction 3 hours.
(4) starch slurry PH7.5 is adjusted, keeping reaction temperature is 30 DEG C, and sodium hypochlorite 30g, the reaction was continued 3h is added.
(5) 10%HCl is added, neutralizes starch slurry, adjusts pH5.2.
(6) it washs, be dehydrated, is dry, out powder.
Embodiment three
In the present embodiment, the dedicated crosslinking -ester-oxidation ternary compound modified starch production method of Wall paper adhesive is as follows:
(1) claim 100g tapioca, be packed into reactor tank, 120g water is added and is dispersed with stirring into uniform starch slurry, will react
Tank moves into the water-bath with blender, starts to stir, water-bath is warming up to slurry temperature up to 38 DEG C.
(2) 2.5%NaOH is added and adjusts starch slurry pH11, sodium trimetaphosphate 0.5g is added, react 3 hours.
(3) 10%HCL is added and adjusts starch slurry pH8.5, adjusting reaction temperature is 28 DEG C, vinylacetate 7g is added, after
Continuous reaction 2 hours.
(4) starch slurry PH7.3 is adjusted, keeping reaction temperature is 28 DEG C, and sodium hypochlorite 15g, the reaction was continued 2h is added.
(5) 10%HCl is added, neutralizes starch slurry, adjusts pH5.1.
(6) it washs, be dehydrated, is dry, out powder.
Embodiment 4
Embodiment three
In the present embodiment, the dedicated crosslinking -ester-oxidation ternary compound modified starch production method of Wall paper adhesive is as follows:
(1) claim 100g tapioca, be packed into reactor tank, 120g water is added and is dispersed with stirring into uniform starch slurry, will react
Tank moves into the water-bath with blender, starts to stir, water-bath is warming up to slurry temperature up to 38 DEG C.
(2) 2.5%NaOH is added and adjusts starch slurry pH11, sodium trimetaphosphate 0.5g is added, react 3 hours.
(3) 10%HCL is added and adjusts starch slurry pH8.5, adjusting reaction temperature is 28 DEG C, vinylacetate 7g is added, after
Continuous reaction 2 hours.
(4) starch slurry PH7.3 is adjusted, keeping reaction temperature is 28 DEG C, and sodium hypochlorite 15g, the reaction was continued 2h is added.
(5) 10%HCl is added, neutralizes starch slurry, adjusts pH5.1.
(6) it washs, Wong Kam-po tree extracting solution is added into dextrin after washing, additive amount is that every 100g adds 50mL.Institute
State the extracting method of Wong Kam-po tree extracting solution are as follows: the branches and leaves for crushing Wong Kam-po tree are put into impregnated 10 days in ethyl alcohol after be obtained by filtration and mention
Take liquid, the weight ratio of Wong Kam-po tree branches and leaves and ethyl alcohol is 1:2.It is finally dehydrated, is dry, out powder.
Comparative example one
In this comparative example, Wall paper adhesive the preparation method is as follows:
By weight, raw material additional amount are as follows: 20 parts of polyvinyl alcohol, 80 parts of cornstarch, 0.2 part of ammonium persulfate.Specific step
Rapid as follows: in a certain amount of water, addition polyvinyl alcohol stirring is warming up to 90 DEG C and makes it completely dissolved, and 60min is stirred, wait cool down
To 60 DEG C of addition ammonium persulfates, 10min is stirred, cornstarch is added, is stirring evenly and then adding into sodium trimetaphosphate and water-bath adds
Heat is warming up to 36 DEG C, reacts 4h；
Tackifier, preservative, plasticizer are added after reaction, stirs evenly, is down to room temperature up to Wall paper adhesive.
Comparative example two
In this comparative example, the dedicated crosslinking -ester-oxidation ternary compound modified starch production method of Wall paper adhesive is as follows:
By weight, raw material additional amount are as follows: 30 parts of polyvinyl alcohol, 70 parts of tapioca, 0.2 part of ammonium persulfate.Specific step
Rapid as follows: in a certain amount of water, addition polyvinyl alcohol stirring is warming up to 90 DEG C and makes it completely dissolved, and 60min is stirred, wait cool down
To 60 DEG C of addition ammonium persulfates, 10min is stirred, tapioca is added, is stirring evenly and then adding into sodium trimetaphosphate and water-bath adds
Heat is warming up to 38 DEG C, reacts 5h；
Tackifier, preservative, plasticizer are added after reaction, stirs evenly, is down to room temperature up to Wall paper adhesive.
Comparative example three
In the present embodiment, the dedicated crosslinking -ester-oxidation ternary compound modified starch production method of Wall paper adhesive is as follows:
By weight, raw material additional amount are as follows: 40 parts of polyvinyl alcohol, 60 parts of potato starch, 0.2 part of ammonium persulfate.Specifically
Steps are as follows: in a certain amount of water, addition polyvinyl alcohol stirring is warming up to 90 DEG C and makes it completely dissolved, and 60min is stirred, wait drop
Temperature stirs 10min, adds potato starch, be stirring evenly and then adding into sodium trimetaphosphate and water to 60 DEG C of addition ammonium persulfates
Bath heating, is warming up to 40 DEG C, reacts 6h；
Tackifier, preservative, plasticizer are added after reaction, stirs evenly, is down to room temperature up to Wall paper adhesive.
The sample number consecutively that embodiment one to three and comparative example one to three are obtained is 1-6, carries out viscosity test and jelly
Melt loop test.
Viscosity test
6 parts of samples are performed the following operation respectively: taking 3g sample and 25g distilled water to be mixed in container, stirs evenly,
Viscosity is measured in viscosimeter.
1 viscosity test results of table
As can be known from the above table, converted starch made from embodiment one to three is as Wall paper adhesive, and viscosity is compared with prior art
Slightly advantage.
Freeze-thaw cycle test
6 parts of samples are performed the following operation respectively: weighing a certain amount of sample, are made into the molten of 5% (w/w, in terms of butt)
Liquid after being heated to 95 DEG C, keeps the temperature 15min, is cooled to room temperature, obtains pasty liquid.
Weigh 50mL centrifuge tube quality (m1), it takes 20g pasty liquid to pour into centrifuge tube, weighs quality (m2).Centrifuge tube is put
Enter in -10~-20 DEG C of refrigerator, is taken out after freezing diel, natural thaw, as a Frozen-thawed cycled.
After 5 Frozen-thawed cycleds, it is centrifuged 20min under the conditions of 6000/min, discards supernatant liquid, weighs sediment quality
(m3), calculate syneresis rate.
Syneresis rate (%)=(m3-m1)/(m2-m1) × 100%
2 freeze-thaw cycle test result of table
As can be seen from Table 2, converted starch made from embodiment one to three is as Wall paper adhesive, and syneresis rate is than comparative example one
Syneresis rate to Wall paper adhesive made from three is small, illustrates preparation method of the invention, can be effectively reduced converted starch finished product
Syneresis rate, reduce starch coagulate limb structure rupture, inhibit frozen-thaw process in starch retrogradation.Denaturation after 5 freeze thawing
Finished product of starch still keeps lower syneresis rate, illustrates that its freeze-thaw stability is higher.
For preferred embodiment (embodiment 3), freeze proof sex determination: converted starch continuously freezes 3 days at -18 DEG C, then thaws,
Observation state.It is further continued for taking out after freezing 3 days and thaw.It is repeated several times, until age of starch is discharged.-ester starch is crosslinked second
Aging after secondary defrosting.Crosslinking -ester-oxidation ternary compound modified starch still maintains good gluing shape after third time is thawed
State.Transparency determines: 1% gelatinized corn starch is the light transmittance at 620nm in wavelength at 25 DEG C.It is crosslinked the light transmittance of -ester starch
It is 5.5%, crosslinking -ester-oxidation ternary compound modified starch light transmittance is 15.0%.
In addition, to embodiment 4 carry out metope coating discovery, after being moistened will not it is mouldy, colloid is not muddy.Illustrate addition
Wong Kam-po tree extract has the function of antibacterial and inhibits fungus breeding.
Use above specific case is illustrated the present invention, is merely used to help understand the present invention, not to limit
The system present invention.For those skilled in the art, according to the thought of the present invention, can also make several simple
It deduces, deform or replaces.
Claims (8)
1. a kind of dedicated cross-linked esterification of Wall paper adhesive aoxidizes ternary compound modified starch production method, it is characterised in that: it includes step
It is rapid: using tapioca as raw material, use respectively crosslinking agent sodium trimetaphosphate, epoxychloropropane, in phosphorus oxychloride at least
A kind of, esterifying agent vinylacetate or acetic anhydride and oxidizing agent sodium hypochlorite carry out reaction of degeneration (RD) to starch, prepare a kind of multiple
Close converted starch.
2. the dedicated cross-linked esterification of a kind of Wall paper adhesive according to claim 1 aoxidizes ternary compound modified starch production method,
It is characterized by: sodium hypochlorite dosage is 10-30g.
3. the dedicated cross-linked esterification of a kind of Wall paper adhesive according to claim 1 aoxidizes ternary compound modified starch production method,
It is characterized by: the dosage of sodium trimetaphosphate is the 0.01-1g of starch on dry basis quality.
4. the dedicated cross-linked esterification of a kind of Wall paper adhesive according to claim 1 aoxidizes ternary compound modified starch production method,
It is characterized by: the dosage of vinylacetate is the 5-10g of starch on dry basis quality.
5. the dedicated cross-linked esterification of a kind of Wall paper adhesive according to claim 1 aoxidizes ternary compound modified starch production method,
It is characterized by: the specific steps of preparation method include:
(1) claim 100g tapioca, be packed into reactor tank, 120g water is added and is dispersed with stirring into uniform starch slurry, reactor tank is moved
Enter in the water-bath with blender, stirring, water-bath is warming up to slurry temperature up to 35-40 DEG C；
(2) 2.5%NaOH is added and adjusts starch slurry to pH10.5-11.5, sodium trimetaphosphate, epoxychloropropane, trichlorine oxygen is added
At least one of phosphorus 0.01-1g reacts 1-5 hours；
(3) 10%HCL is added and adjusts starch slurry to pH8.0-9.0, adjusting reaction temperature is 25-30 DEG C, and vinylacetate is added
Or acetic anhydride 5-10g, the reaction was continued 1-3 hours；
(4) starch slurry PH7.0-7.5 is adjusted, keeping reaction temperature is 25-30 DEG C, sodium hypochlorite 10-30g is added, the reaction was continued
1-3h；
(5) 10%HCl is added, neutralizes starch slurry, is adjusted to pH5.0-5.2；
(6) it washs, be dehydrated, is dry, out powder.
6. the dedicated cross-linked esterification of a kind of Wall paper adhesive according to claim 5 aoxidizes ternary compound modified starch production method,
It is characterized by: water temperature is 36-40 DEG C in heating water bath.
7. the dedicated cross-linked esterification of a kind of Wall paper adhesive according to claim 6 aoxidizes ternary compound modified starch production method,
It is characterized by: Wong Kam-po tree extracting solution is added into dextrin after washing, additive amount is that every 100g adds 50mL.
8. the dedicated cross-linked esterification of a kind of Wall paper adhesive according to claim 7 aoxidizes ternary compound modified starch production method,
It is characterized by: the extracting method of the Wong Kam-po tree extracting solution are as follows: the branches and leaves for crushing Wong Kam-po tree, which are put into ethyl alcohol, impregnates 10
It is obtained by filtration extracting solution after it, the weight ratio of Wong Kam-po tree branches and leaves and ethyl alcohol is 1:2.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112111017A (en) * | 2020-09-03 | 2020-12-22 | 绿色轻化科技发展(北京)有限公司 | Degradable cassava acetate starch, resin thereof, preparation method and application of degradable cassava acetate starch and resin |
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| CN101045752A (en) * | 2007-04-29 | 2007-10-03 | 江苏技术师范学院 | Preparation method of oxidation cross-linked esterification triple modified starch |
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| CN101045752A (en) * | 2007-04-29 | 2007-10-03 | 江苏技术师范学院 | Preparation method of oxidation cross-linked esterification triple modified starch |
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| CN112111017A (en) * | 2020-09-03 | 2020-12-22 | 绿色轻化科技发展(北京)有限公司 | Degradable cassava acetate starch, resin thereof, preparation method and application of degradable cassava acetate starch and resin |
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Application publication date: 20190222 |