CN105524575A - Preparation method of esterified lotus root starch/polyvinyl alcohol blend adhesive - Google Patents
Preparation method of esterified lotus root starch/polyvinyl alcohol blend adhesive Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B21/00—Layered products comprising a layer of wood, e.g. wood board, veneer, wood particle board
- B32B21/13—Layered products comprising a layer of wood, e.g. wood board, veneer, wood particle board all layers being exclusively wood
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/06—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the heating method
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/10—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the pressing technique, e.g. using action of vacuum or fluid pressure
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/12—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by using adhesives
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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
- 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
- C08F8/00—Chemical modification by after-treatment
- C08F8/28—Condensation with aldehydes or ketones
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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
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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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
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
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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
- C09J129/00—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Adhesives based on hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Adhesives based on derivatives of such polymers
- C09J129/14—Homopolymers or copolymers of acetals or ketals obtained by polymerisation of unsaturated acetals or ketals or by after-treatment of polymers of unsaturated alcohols
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Polymers & Plastics (AREA)
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- Medicinal Chemistry (AREA)
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- Biochemistry (AREA)
- Physics & Mathematics (AREA)
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- General Chemical & Material Sciences (AREA)
- Wood Science & Technology (AREA)
- Inorganic Chemistry (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The invention discloses a preparation method of an esterified lotus root starch/polyvinyl alcohol blend adhesive, and belongs to the field of adhesives. Lotus root starch is esterified to reduce starch intermolecular polarity, so the dissolvability and the chemical stability of the starch are improved; and the esterified starch is added to a polyvinyl alcohol adhesive, so the waterproof and mechanical performances of polyvinyl alcohol are improved, and the blend adhesive prepared in the invention is green and environmentally-friendly, and causes no pungent odor or toxicity.
Description
Technical field
The invention discloses the preparation method of a kind of esterification Lotus Root Starch/polyvinyl alcohol blending sizing agent, belong to sizing agent field.
Background technology
Polyvinyl alcohol is a kind of purposes water-soluble polymer very widely, unique properties, by in a large number for the production of manufacture coating, emulsifying agent, tackiness agent, textiles, the products such as paper product machining agent and plastics film, as one development thermosol very fast, it has good strong adherence, tough and tensile transparent, glued membrane intensity is high, oil resistant, corrosion resistant is lit up, solvent resistant, wear-resisting, and there is good barrier properties for gases and thermostability, be applicable to wood-based plate, core-board, glued board, shaving board, high density fiberboard etc. bonding, there is manufacturing process simple, the feature that curing speed is fast.But the high molecular speciality of water-soluble polyhydroxyl makes polyvinyl alcohol based Wood Adhesives have poor water resistance, thus limits its range of application.At present, people often adopt interpolation formaldehyde, butyraldehyde or crotonaldehyde to make polyvinyl alcohol acetalation, interpolation tolylene diisocyanate or triphenylmethane triisocyanate carry out cross-linking modified method to improve water tolerance and the adhesiveproperties of polyvinyl alcohol glue to polyvinyl alcohol, achieve obvious modified effect, but due to pungent odour and the toxicity of aldehydes and isocyanic ester, its application is affected.In addition, also can adopt and add the method such as wood fibre, nano clay to improve water tolerance and the mechanical property of polyvinyl alcohol, but these method of modifying to there is operating procedure more complicated, introduce the problem that the cost of raw material is higher.
Starch has many advantages, but starch is a kind of crystal material of strong polarity, in molecule, there is a large amount of hydrogen bond, under general condition with intermolecular, the fat-soluble difference of native starch, stick with paste liquid unstable under acid, heat, shearing action, be difficult to machine-shaping, be insoluble to cold water, therefore, in order to meet certain needs, starch, frequently by chemical modification, changes its physics and other character.Containing glycosidic link and the light base of activity in starch molecule, can and many material generation chemical reactions, be the basis of starch being carried out to chemical modification, wherein oxidation, esterification, etherificate, be cross-linked, grafting etc. is conventional chemical modification method.
Summary of the invention
The technical problem that the present invention mainly solves: there is poor water resistance for current polyvinyl alcohol based Wood Adhesives, and be affected because the pungent odour of aldehydes and isocyanic ester and toxicity make it apply, and the fat-soluble difference of native starch, stick with paste liquid in acid, heat, unstable under shearing action, be difficult to the problem of machine-shaping, provide the preparation method of a kind of esterification Lotus Root Starch-polyvinyl alcohol blending sizing agent, Lotus Root Starch is carried out esterification modification by the present invention, reduce starch molecule intermediate polarity, thus improve solvability and the chemical stability of starch, starch after esterification is added in the agent of polyvinyl alcohol gluing, not only can improve water tolerance and the mechanical property of polyvinyl alcohol, and obtained blended sizing agent environmental protection, pungent odour and toxicity can not be produced.
In order to solve the problems of the technologies described above, the technical solution adopted in the present invention is:
(1) take 200 ~ 250g Lotus Root Starch and be placed in 1000mL reactor with whipping appts, 8 ~ 15mL massfraction 35% sodium hydroxide solution is added successively again in still, 40 ~ 60mL dehydrated alcohol and 200 ~ 300mL deionized water, reactor be warming up to 35 ~ 45 DEG C and be uniformly mixed, the starch milk obtained after stirring is poured in beaker, and processing by ultrasonic wave, 15 ~ 20min is processed under ultrasonic power is 700 ~ 850W, starch milk after process is carried out centrifugation, taking precipitate puts into 45 ~ 55 DEG C of constant temperature ovens, and to be dried to water content be 5 ~ 8%, taking-up is put into pulverizer and is pulverized, sieve to obtain 200 ~ 220 order powder,
(2) the above-mentioned starch powder of 100 ~ 120g and 10 ~ 15g esterifying agent maleic anhydride is got, massfraction 85% aqueous ethanolic solution is added wherein again by solid-to-liquid ratio 1:1.3, 2 ~ 3g catalyzer urea is added again after stirring, and be 5 ~ 6 by massfraction 35% formic acid solution adjust ph, starch esterification reaction 1 ~ 2h is carried out at temperature is 45 ~ 60 DEG C, 5 ~ 8g tensio-active agent fatty alcohol-polyoxyethylene ether is added again after reaction terminates, filter after stirring, filter residue is used deionized water respectively, acetone and absolute ethanol washing filter 2 ~ 3 times, get filter cake and carry out drying, dry completely rear pulverizing, sieve to obtain 150 ~ 180 order powder, powder is placed in microwave reactor, setting microwave power power is 800 ~ 1200W, esterification Lotus Root Starch is taken out to obtain after process 5 ~ 8min, for subsequent use,
(3) 50 ~ 80g polyvinyl alcohol is taken in the there-necked flask of 1000mL, 300 ~ 350mL massfraction 35% formalin is added respectively again in bottle, put into water bath with thermostatic control, raised temperature to 85 ~ 95 DEG C, and stir until solid dissolves completely, temperature to 30 ~ 40 DEG C are reduced after dissolving, the hydrochloric acid soln adjust ph dripping 37% is 4.5 ~ 5.5, taking 2 ~ 3g S-WAT after adjustment again adds wherein, insulated and stirred reaction 40 ~ 50min, reaction terminates rear dropping 3 ~ 5 polypropylene glycerol aether defoamers, stir cool to room temperature, pH is regulated to be 7.0 with massfraction 15% sodium hydroxide solution, obtain polyvinyl alcohol sizing agent,
(4) 20 ~ 30g step (2) esterification Lotus Root Starch is got, above-mentioned obtained polyvinyl alcohol sizing agent and total mass 0.5 ~ 0.8% ammonium persulphate, 1 ~ 3% polysiloxane, 5 ~ 8% massfraction 15% borax solns are added wherein by solid-to-liquid ratio 1:1.5, stir at 30 ~ 35 DEG C, stop stirring until muddy glue becomes translucent glue, leave standstill to deaeration and can obtain blended sizing agent completely.
Application method of the present invention: getting a veneer is dash board, its surface uniform is smeared the blended sizing agent that one deck the present invention obtains, after natural air drying 30 ~ 40s, getting another veneer is again central layer, by fiber direction and first veneer mutually vertically superposed, at the upper surface blended sizing agent of uniform application again, natural air drying 30 ~ 40s, get the 3rd veneer vertical with central layer and contact overlap with loose side with central layer glue face by its fiber direction, combination completes, hot-forming process 8 ~ 15min is carried out under 140 ~ 170 DEG C and 1.2 ~ 2.0MPa, be cooled to room temperature again, coldmoulding process 5 ~ 10min is carried out under 1.1 ~ 1.5MPa pressure, .
The invention has the beneficial effects as follows:
(1) Lotus Root Starch is carried out esterification modification by the present invention, reduces starch molecule intermediate polarity, improves solvability and the chemical stability of starch, is added on by starch after esterification in the agent of polyvinyl alcohol gluing, not only can improves water tolerance and the mechanical property of polyvinyl alcohol;
(2) the sizing agent environmental protection that obtains of the present invention, can not produce pungent odour and toxicity.
Embodiment
First take 200 ~ 250g Lotus Root Starch and be placed in 1000mL reactor with whipping appts, 8 ~ 15mL massfraction 35% sodium hydroxide solution is added successively again in still, 40 ~ 60mL dehydrated alcohol and 200 ~ 300mL deionized water, reactor be warming up to 35 ~ 45 DEG C and be uniformly mixed, the starch milk obtained after stirring is poured in beaker, and processing by ultrasonic wave, 15 ~ 20min is processed under ultrasonic power is 700 ~ 850W, starch milk after process is carried out centrifugation, taking precipitate puts into 45 ~ 55 DEG C of constant temperature ovens, and to be dried to water content be 5 ~ 8%, taking-up is put into pulverizer and is pulverized, sieve to obtain 200 ~ 220 order powder,
Get the above-mentioned starch powder of 100 ~ 120g and 10 ~ 15g esterifying agent maleic anhydride, massfraction 85% aqueous ethanolic solution is added wherein again by solid-to-liquid ratio 1:1.3, 2 ~ 3g catalyzer urea is added again after stirring, and be 5 ~ 6 by massfraction 35% formic acid solution adjust ph, starch esterification reaction 1 ~ 2h is carried out at temperature is 45 ~ 60 DEG C, 5 ~ 8g tensio-active agent fatty alcohol-polyoxyethylene ether is added again after reaction terminates, filter after stirring, filter residue is used deionized water respectively, acetone and absolute ethanol washing filter 2 ~ 3 times, get filter cake and carry out drying, dry completely rear pulverizing, sieve to obtain 150 ~ 180 order powder, powder is placed in microwave reactor, setting microwave power power is 800 ~ 1200W, esterification Lotus Root Starch is taken out to obtain after process 5 ~ 8min, for subsequent use, take 50 ~ 80g polyvinyl alcohol in the there-necked flask of 1000mL, 300 ~ 350mL massfraction 35% formalin is added respectively again in bottle, put into water bath with thermostatic control, raised temperature to 85 ~ 95 DEG C, and stir until solid dissolves completely, temperature to 30 ~ 40 DEG C are reduced after dissolving, the hydrochloric acid soln adjust ph dripping 37% is 4.5 ~ 5.5, taking 2 ~ 3g S-WAT after adjustment again adds wherein, insulated and stirred reaction 40 ~ 50min, reaction terminates rear dropping 3 ~ 5 polypropylene glycerol aether defoamers, stir cool to room temperature, pH is regulated to be 7.0 with massfraction 15% sodium hydroxide solution, obtain polyvinyl alcohol sizing agent, get 20 ~ 30g esterification Lotus Root Starch, above-mentioned obtained polyvinyl alcohol sizing agent and total mass 0.5 ~ 0.8% ammonium persulphate, 1 ~ 3% polysiloxane, 5 ~ 8% massfraction 15% borax solns are added wherein by solid-to-liquid ratio 1:1.5, stir at 30 ~ 35 DEG C, stop stirring until muddy glue becomes translucent glue, leave standstill to deaeration and can obtain blended sizing agent completely.
Example 1
First take 200g Lotus Root Starch and be placed in 1000mL reactor with whipping appts, 8mL massfraction 35% sodium hydroxide solution is added successively again in still, 40mL dehydrated alcohol and 200mL deionized water, reactor be warming up to 35 DEG C and be uniformly mixed, the starch milk obtained after stirring is poured in beaker, and processing by ultrasonic wave, 15min is processed under ultrasonic power is 700W, starch milk after process is carried out centrifugation, taking precipitate puts into 45 DEG C of constant temperature ovens, and to be dried to water content be 5%, taking-up is put into pulverizer and is pulverized, sieve to obtain 200 order powder, get the above-mentioned starch powder of 100g and 10g esterifying agent maleic anhydride, massfraction 85% aqueous ethanolic solution is added wherein again by solid-to-liquid ratio 1:1.3, 2g catalyzer urea is added again after stirring, and be 5 by massfraction 35% formic acid solution adjust ph, starch esterification reaction 1h is carried out at temperature is 45 DEG C, 5g tensio-active agent fatty alcohol-polyoxyethylene ether is added again after reaction terminates, filter after stirring, filter residue is used deionized water respectively, acetone and absolute ethanol washing filter 2 times, get filter cake and carry out drying, dry completely rear pulverizing, sieve to obtain 150 order powder, powder is placed in microwave reactor, setting microwave power power is 800W, esterification Lotus Root Starch is taken out to obtain after process 5min, for subsequent use, take 50g polyvinyl alcohol in the there-necked flask of 1000mL, 300mL massfraction 35% formalin is added respectively again in bottle, put into water bath with thermostatic control, raised temperature to 85 DEG C, and stir until solid dissolves completely, temperature to 30 DEG C is reduced after dissolving, the hydrochloric acid soln adjust ph dripping 37% is 4.5, taking 2g S-WAT after adjustment again adds wherein, insulated and stirred reaction 40min, reaction terminates rear dropping 3 polypropylene glycerol aether defoamers, stir cool to room temperature, pH is regulated to be 7.0 with massfraction 15% sodium hydroxide solution, obtain polyvinyl alcohol sizing agent, get 20g esterification Lotus Root Starch, above-mentioned obtained polyvinyl alcohol sizing agent and total mass 0.5% ammonium persulphate, 1% polysiloxane, 5% massfraction 15% borax soln is added wherein by solid-to-liquid ratio 1:1.5, stir at 30 DEG C, stop stirring until muddy glue becomes translucent glue, leave standstill to deaeration and can obtain blended sizing agent completely.
Getting a veneer is dash board, its surface uniform is smeared the blended sizing agent that one deck the present invention obtains, after natural air drying 30s, getting another veneer is again central layer, by fiber direction and first veneer mutually vertically superposed, at the upper surface blended sizing agent of uniform application again, natural air drying 30s, get the 3rd veneer vertical with central layer and contact overlap with loose side with central layer glue face by its fiber direction, combination completes, and carries out hot-forming process 8min, then be cooled to room temperature under 140 DEG C and 1.2MPa, coldmoulding process 5min is carried out under 1.1MPa pressure.
Example 2
First take 225g Lotus Root Starch and be placed in 1000mL reactor with whipping appts, 12mL massfraction 35% sodium hydroxide solution is added successively again in still, 50mL dehydrated alcohol and 250mL deionized water, reactor be warming up to 40 DEG C and be uniformly mixed, the starch milk obtained after stirring is poured in beaker, and processing by ultrasonic wave, 17min is processed under ultrasonic power is 770W, starch milk after process is carried out centrifugation, taking precipitate puts into 50 DEG C of constant temperature ovens, and to be dried to water content be 6%, taking-up is put into pulverizer and is pulverized, sieve to obtain 210 order powder, get the above-mentioned starch powder of 110g and 13g esterifying agent maleic anhydride, massfraction 85% aqueous ethanolic solution is added wherein again by solid-to-liquid ratio 1:1.3, 2.5g catalyzer urea is added again after stirring, and be 5.5 by massfraction 35% formic acid solution adjust ph, starch esterification reaction 1.5h is carried out at temperature is 52 DEG C, 6g tensio-active agent fatty alcohol-polyoxyethylene ether is added again after reaction terminates, filter after stirring, filter residue is used deionized water respectively, acetone and absolute ethanol washing filter 2 times, get filter cake and carry out drying, dry completely rear pulverizing, sieve to obtain 165 order powder, powder is placed in microwave reactor, setting microwave power power is 1000W, esterification Lotus Root Starch is taken out to obtain after process 7min, for subsequent use, take 65g polyvinyl alcohol in the there-necked flask of 1000mL, 325mL massfraction 35% formalin is added respectively again in bottle, put into water bath with thermostatic control, raised temperature to 90 DEG C, and stir until solid dissolves completely, temperature to 35 DEG C is reduced after dissolving, the hydrochloric acid soln adjust ph dripping 37% is 5.0, taking 2.5g S-WAT after adjustment again adds wherein, insulated and stirred reaction 45min, reaction terminates rear dropping 4 polypropylene glycerol aether defoamers, stir cool to room temperature, pH is regulated to be 7.0 with massfraction 15% sodium hydroxide solution, obtain polyvinyl alcohol sizing agent, get 25g esterification Lotus Root Starch, above-mentioned obtained polyvinyl alcohol sizing agent and total mass 0.7% ammonium persulphate, 2% polysiloxane, 7% massfraction 15% borax soln is added wherein by solid-to-liquid ratio 1:1.5, stir at 33 DEG C, stop stirring until muddy glue becomes translucent glue, leave standstill to deaeration and can obtain blended sizing agent completely.
Getting a veneer is dash board, its surface uniform is smeared the blended sizing agent that one deck the present invention obtains, after natural air drying 35s, getting another veneer is again central layer, by fiber direction and first veneer mutually vertically superposed, at the upper surface blended sizing agent of uniform application again, natural air drying 35s, get the 3rd veneer vertical with central layer and contact overlap with loose side with central layer glue face by its fiber direction, combination completes, and carries out hot-forming process 12min, then be cooled to room temperature under 155 DEG C and 1.6MPa, coldmoulding process 8min is carried out under 1.3MPa pressure.
Example 3
First take 250g Lotus Root Starch and be placed in 1000mL reactor with whipping appts, 15mL massfraction 35% sodium hydroxide solution is added successively again in still, 60mL dehydrated alcohol and 300mL deionized water, reactor be warming up to 45 DEG C and be uniformly mixed, the starch milk obtained after stirring is poured in beaker, and processing by ultrasonic wave, 20min is processed under ultrasonic power is 850W, starch milk after process is carried out centrifugation, taking precipitate puts into 55 DEG C of constant temperature ovens, and to be dried to water content be 8%, taking-up is put into pulverizer and is pulverized, sieve to obtain 220 order powder, get the above-mentioned starch powder of 120g and 15g esterifying agent maleic anhydride, massfraction 85% aqueous ethanolic solution is added wherein again by solid-to-liquid ratio 1:1.3, 3g catalyzer urea is added again after stirring, and be 6 by massfraction 35% formic acid solution adjust ph, starch esterification reaction 2h is carried out at temperature is 60 DEG C, 8g tensio-active agent fatty alcohol-polyoxyethylene ether is added again after reaction terminates, filter after stirring, filter residue is used deionized water respectively, acetone and absolute ethanol washing filter 23, get filter cake and carry out drying, dry completely rear pulverizing, sieve to obtain 180 order powder, powder is placed in microwave reactor, setting microwave power power is 1200W, esterification Lotus Root Starch is taken out to obtain after process 8min, for subsequent use, take 80g polyvinyl alcohol in the there-necked flask of 1000mL, 350mL massfraction 35% formalin is added respectively again in bottle, put into water bath with thermostatic control, raised temperature to 95 DEG C, and stir until solid dissolves completely, temperature to 40 DEG C is reduced after dissolving, the hydrochloric acid soln adjust ph dripping 37% is 5.5, taking 3g S-WAT after adjustment again adds wherein, insulated and stirred reaction 50min, reaction terminates rear dropping 5 polypropylene glycerol aether defoamers, stir cool to room temperature, pH is regulated to be 7.0 with massfraction 15% sodium hydroxide solution, obtain polyvinyl alcohol sizing agent, get 30g esterification Lotus Root Starch, above-mentioned obtained polyvinyl alcohol sizing agent and total mass 0.8% ammonium persulphate, 3% polysiloxane, 8% massfraction 15% borax soln is added wherein by solid-to-liquid ratio 1:1.5, stir at 35 DEG C, stop stirring until muddy glue becomes translucent glue, leave standstill to deaeration and can obtain blended sizing agent completely.
Getting a veneer is dash board, surface uniform is smeared one deck the present invention and obtain blended sizing agent, natural air drying 40s, getting another veneer is again central layer, by fiber direction and first veneer mutually vertically superposed, at the upper surface blended sizing agent of uniform application again, natural air drying 40s, get the 3rd veneer vertical with central layer and contact overlap with loose side with central layer glue face by its fiber direction, combination completes, and carries out hot-forming process 15min, then be cooled to room temperature under 170 DEG C and 2.0MPa, coldmoulding process 10min is carried out under 1.5MPa pressure.
Claims (1)
1. a preparation method for esterification Lotus Root Starch/polyvinyl alcohol blending sizing agent, is characterized in that concrete preparation process is:
(1) take 200 ~ 250g Lotus Root Starch and be placed in 1000mL reactor with whipping appts, 8 ~ 15mL massfraction 35% sodium hydroxide solution is added successively again in still, 40 ~ 60mL dehydrated alcohol and 200 ~ 300mL deionized water, reactor be warming up to 35 ~ 45 DEG C and be uniformly mixed, the starch milk obtained after stirring is poured in beaker, and processing by ultrasonic wave, 15 ~ 20min is processed under ultrasonic power is 700 ~ 850W, starch milk after process is carried out centrifugation, taking precipitate puts into 45 ~ 55 DEG C of constant temperature ovens, and to be dried to water content be 5 ~ 8%, taking-up is put into pulverizer and is pulverized, sieve to obtain 200 ~ 220 order powder,
(2) the above-mentioned starch powder of 100 ~ 120g and 10 ~ 15g esterifying agent maleic anhydride is got, massfraction 85% aqueous ethanolic solution is added wherein again by solid-to-liquid ratio 1:1.3, 2 ~ 3g catalyzer urea is added again after stirring, and be 5 ~ 6 by massfraction 35% formic acid solution adjust ph, starch esterification reaction 1 ~ 2h is carried out at temperature is 45 ~ 60 DEG C, 5 ~ 8g tensio-active agent fatty alcohol-polyoxyethylene ether is added again after reaction terminates, filter after stirring, filter residue is used deionized water respectively, acetone and absolute ethanol washing filter 2 ~ 3 times, get filter cake and carry out drying, dry completely rear pulverizing, sieve to obtain 150 ~ 180 order powder, powder is placed in microwave reactor, setting microwave power power is 800 ~ 1200W, esterification Lotus Root Starch is taken out to obtain after process 5 ~ 8min, for subsequent use,
(3) 50 ~ 80g polyvinyl alcohol is taken in the there-necked flask of 1000mL, 300 ~ 350mL massfraction 35% formalin is added respectively again in bottle, put into water bath with thermostatic control, raised temperature to 85 ~ 95 DEG C, and stir until solid dissolves completely, temperature to 30 ~ 40 DEG C are reduced after dissolving, the hydrochloric acid soln adjust ph dripping 37% is 4.5 ~ 5.5, taking 2 ~ 3g S-WAT after adjustment again adds wherein, insulated and stirred reaction 40 ~ 50min, reaction terminates rear dropping 3 ~ 5 polypropylene glycerol aether defoamers, stir cool to room temperature, pH is regulated to be 7.0 with massfraction 15% sodium hydroxide solution, obtain polyvinyl alcohol sizing agent,
(4) 20 ~ 30g step (2) esterification Lotus Root Starch is got, above-mentioned obtained polyvinyl alcohol sizing agent and total mass 0.5 ~ 0.8% ammonium persulphate, 1 ~ 3% polysiloxane, 5 ~ 8% massfraction 15% borax solns are added wherein by solid-to-liquid ratio 1:1.5, stir at 30 ~ 35 DEG C, stop stirring until muddy glue becomes translucent glue, leave standstill to deaeration and can obtain blended sizing agent completely.
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| CN106218056A (en) * | 2016-08-31 | 2016-12-14 | 阜南县天亿工艺品有限公司 | A kind of ferrum skill artware packaging thermal insulation board preparation method |
| CN107384247A (en) * | 2017-07-12 | 2017-11-24 | 马鞍山科信网络科技有限公司 | A kind of based Wood Adhesives based on esterification modification tapioca and preparation method thereof |
| CN107401006A (en) * | 2017-08-14 | 2017-11-28 | 利均刺绣(海宁)有限公司 | A kind of patch anglicanum |
| CN110172105A (en) * | 2019-05-22 | 2019-08-27 | 华南理工大学 | A method of improving dry method/semidry method starch and etherifying agent reaction efficiency |
-
2015
- 2015-12-28 CN CN201510997353.8A patent/CN105524575A/en not_active Withdrawn
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106218056A (en) * | 2016-08-31 | 2016-12-14 | 阜南县天亿工艺品有限公司 | A kind of ferrum skill artware packaging thermal insulation board preparation method |
| CN107384247A (en) * | 2017-07-12 | 2017-11-24 | 马鞍山科信网络科技有限公司 | A kind of based Wood Adhesives based on esterification modification tapioca and preparation method thereof |
| CN107401006A (en) * | 2017-08-14 | 2017-11-28 | 利均刺绣(海宁)有限公司 | A kind of patch anglicanum |
| CN110172105A (en) * | 2019-05-22 | 2019-08-27 | 华南理工大学 | A method of improving dry method/semidry method starch and etherifying agent reaction efficiency |
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