CN106496908A - A kind of preparation method of water soluble core-mould material - Google Patents
A kind of preparation method of water soluble core-mould material Download PDFInfo
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- CN106496908A CN106496908A CN201610870358.9A CN201610870358A CN106496908A CN 106496908 A CN106496908 A CN 106496908A CN 201610870358 A CN201610870358 A CN 201610870358A CN 106496908 A CN106496908 A CN 106496908A
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- starch
- water soluble
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Classifications
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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
- C08L51/00—Compositions of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers
- C08L51/02—Compositions of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers grafted on to polysaccharides
-
- 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
- C08F251/00—Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/24—Crosslinking, e.g. vulcanising, of macromolecules
- C08J3/246—Intercrosslinking of at least two polymers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2351/00—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers
- C08J2351/02—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers grafted on to polysaccharides
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2489/00—Characterised by the use of proteins; Derivatives thereof
-
- 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
Abstract
The present invention relates to a kind of preparation method of water soluble core-mould material, belongs to core technical field of material.For existing water soluble starch core material, mechanical property is relatively low, the larger problem for easily causing stress concentration of modified filler density, provide a kind of preparation method of water soluble core-mould material, the present invention passes through modification of corn starch graft cyanoethyl group, make its hydrophobically modified, reduce its starch cross-link intensity, strengthen its water soluble characteristic, albumen is separated to its compound soybean simultaneously, modified starch mechanical strength, subsequently carried out by tiny balloon composite filled, while starch-based water-soluble core material is effectively improved, reduce the problem that stress concentration filled by filler.Water soluble core-mould material compressive strength prepared by the present invention improves 25～30% compared with like product, and filler conjugation is higher, and water solubility rate improves 10～15%, and preparation process is simple, is prepared by starch, and green safety is pollution-free.
Description
Technical field
The present invention relates to a kind of preparation method of water soluble core-mould material, belongs to core technical field of material.
Background technology
Water soluble core-mould material, is referred to and is bonded together some fillers by various water soluble adhesives, and according to making
With requiring to make, tool is effigurate, there is in using temperature range certain mechanical property and can keep shape,
Make which defeated and dispersed using water equal solvent during the demoulding then the demoulding obtain product a kind of composite.Water soluble core-mould material due to into
The features such as type high precision, low cost, efficiency high, easy mold release, the casting sternly required in various high standards and composite manufacture work
Obtain a wide range of applications in industry.As the starch family macromolecule of traditional water soluble adhesive, with nonhazardouss, pollution-free etc.
Feature, while filming performance is good, with excellent bond propertiess, collapsibility is good, be a kind of have a extensive future natural water-soluble
Property adhesive.
As the starch family macromolecule of traditional water soluble adhesive, with nonhazardouss, pollution-free the features such as, while film forming
Performance is good, and with excellent bond propertiess, collapsibility is good, is a kind of water-soluble adhesive having a extensive future.But
Due to the deficiency of its mechanical property, the research for making starch family macromolecule be used as water soluble core-mould material once stayed cool.
Meanwhile, the improvement to water soluble core-mould material in the past, mainly around to using the exploitation of adhesive carry out, and to core
The research of the filler that mold materialss are used is paid attention to not enough.This also limit the development of core material to a certain extent.Tradition is used
Filler due to there are problems that density is larger, in irregular shape, easily causing, be difficult to meet some high-performance
Therefore the use requirement of core material, prepares a kind of core material of high-strength performance necessary.
Content of the invention
The technical problem to be solved：For existing water soluble starch core material, mechanical property is relatively low, change
Property the larger problem for easily causing stress concentration of packing density, there is provided a kind of preparation method of water soluble core-mould material, the present invention
By by modification of corn starch graft cyanoethyl group so as to hydrophobically modified, reduce its starch cross-link intensity so as to which water soluble characteristic increases
By force, while separating albumen to its compound soybean, modified starch mechanical strength, subsequently carried out by tiny balloon composite filled,
While being effectively improved starch-based water-soluble core material, reduce the problem that stress concentration filled by filler.
For solving above-mentioned technical problem, the technical solution used in the present invention is：
（1）In mass ratio 1:5, corn starch is mixed with the stirring of 1% sodium hydroxide solution of mass fraction, water at 35～40 DEG C
Bath 25～30min of heating, subsequently the acrylonitrile monemer of insulation Deca sodium hydroxide quality 30%, controls rate of addition for 1mL/
Min, after being added dropwise to complete, adjusts pH to 5.5 with glacial acetic acid, after 15～20min of insulation reaction, stands and is cooled to room temperature, subsequently
Sucking filtration simultaneously collects filter cake, is washed with deionized 3～5 times, at 45～50 DEG C dries 20～24h, is prepared into modified grafting beautiful
Rice starch, standby；
（2）Count by weight, weigh 45～50 parts of 20% sodium chloride solutions of mass fraction, 10～15 parts of above-mentioned preparations respectively
Modified Grafted Starch, 1～2 part of Hydrazoic acid,sodium salt and 5～10 parts of soybean protein isolates are placed in conical flask, stirring mixing 25
～30min, is evacuated to 10～15Pa and is placed in standing 20～24h at 0～5 DEG C, be prepared into mixed and modified liquid；
（3）By volume 1:1, normal hexane is mixed with the mixed and modified liquid stirring of above-mentioned preparation and is placed in beaker, subsequently right
5% sorbitan fatty ester of Deca normal hexane quality in beaker, stirring mixing are placed in high-speed shearing emulsion machine, are cut
After cutting 10～15min of emulsifying, to adding the polyvinyl alcohol of normal hexane quality 3% in beaker, at 45～50 DEG C stirring mixing 3～
5h, subsequent sucking filtration simultaneously collect filter cake, after being washed with deionized 3～5 times, dry 6～8h, be prepared into crosslinking at 65～70 DEG C
Tiny balloon；
（4）Count by weight, weigh 25～30 parts of crosslinking tiny balloons, 30～35 parts of steps respectively（1）Standby modification connects
Branch corn starch and 10～15 parts of 5% sodium tetraborate solution of mass fraction are placed in beaker, during stirring mixes and pours to mould,
At room temperature, mould is placed in 45～60s of compacting under 25～30MPa, subsequently stands 6～8h of solidification, then do at 65～70 DEG C
Dry 6～8h, is prepared into a kind of water soluble core-mould material by naturally cooling to room temperature.
Water solubility rate is 0.035g/min to water soluble core-mould material prepared by the present invention at room temperature, and comprcssive strength is reachable
9.5～12.0MPa, density are 1.03g/cm3, thermal coefficient of expansion is 3.85 × 10-6/℃-1.
Compared with additive method, Advantageous Effects are the present invention：
（1）The present invention prepare water soluble core-mould material compressive strength compared with like product improve 25～30%, and filler conjugation compared with
Height, water solubility rate improve 10～15%；
（2）Preparation process of the present invention is simple, is prepared by starch, and green safety is pollution-free.
Specific embodiment
First in mass ratio 1:5, corn starch is mixed with the stirring of 1% sodium hydroxide solution of mass fraction, at 35～40 DEG C
25～30min of lower heating in water bath, is subsequently incubated the acrylonitrile monemer of Deca sodium hydroxide quality 30%, and controlling rate of addition is
1mL/min, after being added dropwise to complete, adjusts pH to 5.5 with glacial acetic acid, after 15～20min of insulation reaction, stands and is cooled to room temperature,
Subsequent sucking filtration simultaneously collects filter cake, is washed with deionized 3～5 times, dries 20～24h, be prepared into modification and connect at 45～50 DEG C
Branch corn starch, standby；Count by weight, weigh 45～50 parts of 20% sodium chloride solutions of mass fraction respectively, on 10～15 parts
Modified Grafted Starch, 1～2 part of Hydrazoic acid,sodium salt and 5～10 parts of soybean protein isolates for stating preparation are placed in conical flask, are stirred
25～30min of mixing is mixed, and is evacuated to 10～15Pa and is placed in 20～24h being stood at 0～5 DEG C, is prepared into mixed and modified liquid；Press
Volume ratio 1:1, normal hexane is mixed with the mixed and modified liquid stirring of above-mentioned preparation and is placed in beaker, subsequently to Deca in beaker
5% sorbitan fatty ester of normal hexane quality, stirring mixing are placed in high-speed shearing emulsion machine, and emulsification pretreatment 10～
After 15min, to adding the polyvinyl alcohol of normal hexane quality 3% in beaker, 3～5h of stirring mixing, subsequent sucking filtration at 45～50 DEG C
And filter cake is collected, after being washed with deionized 3～5 times, 6～8h is dried at 65～70 DEG C, be prepared into crosslinking tiny balloon；Press
Parts by weight meter, weighs 25～30 parts of crosslinking tiny balloons, 30～35 parts of steps respectively（1）Standby modified Grafted Starch
It is placed in beaker with 10～15 parts of mass fractions, 5% sodium tetraborate solution, during stirring mixes and pours to mould, at room temperature, will
Mould is placed in 45～60s of compacting under 25～30MPa, subsequently stands 6～8h of solidification, then dries 6～8h at 65～70 DEG C, natural
A kind of water soluble core-mould material is prepared into by being cooled to room temperature.
Example 1
First in mass ratio 1:5, corn starch is mixed with the stirring of 1% sodium hydroxide solution of mass fraction, water-bath at 35 DEG C adds
Hot 25min, subsequently the acrylonitrile monemer of insulation Deca sodium hydroxide quality 30%, controls rate of addition for 1mL/min, treats Deca
After the completion of, pH to 5.5 is adjusted with glacial acetic acid, after insulation reaction 15min, stand and be cooled to room temperature, subsequent sucking filtration simultaneously collects filter cake,
It is washed with deionized 3 times, at 45 DEG C, dries 20h, is prepared into modified Grafted Starch, standby；Count by weight, point
45 parts of 20% sodium chloride solutions of mass fraction of another name amount, the modified Grafted Starch of 10 parts of above-mentioned preparations, 1 part of Hydrazoic acid,sodium salt and 5
Part soybean protein isolate is placed in conical flask, stirring mixing 25min, is evacuated to 10Pa and is placed in standing 20h, system at 0 DEG C
Standby mixed and modified liquid；By volume 1:1, normal hexane is mixed with the mixed and modified liquid stirring of above-mentioned preparation and is placed in beaker
In, subsequently to 5% sorbitan fatty ester of Deca normal hexane quality in beaker, stirring mixing is placed in high speed shear breast
In change machine, after emulsification pretreatment 10min, to adding the polyvinyl alcohol of normal hexane quality 3% in beaker, stirring mixing 3h at 45 DEG C,
Subsequent sucking filtration simultaneously collects filter cake, after being washed with deionized 3 times, dries 6h at 65 DEG C, is prepared into crosslinking tiny balloon；By weight
Amount number meter, weighs 25 parts of crosslinking tiny balloons, 30 parts of modified Grafted Starch and 10 parts of 5% tetraboric acids of mass fraction respectively
Sodium solution is placed in beaker, during stirring mixes and pours to mould, at room temperature, mould is placed in compacting 45s under 25MPa, with
Stand solidification 6h afterwards, then 6h is dried at 65 DEG C, be prepared into a kind of water soluble core-mould material by naturally cooling to room temperature.
Example 2
First in mass ratio 1:5, corn starch is mixed with the stirring of 1% sodium hydroxide solution of mass fraction, water-bath at 37 DEG C adds
Hot 27min, subsequently the acrylonitrile monemer of insulation Deca sodium hydroxide quality 30%, controls rate of addition for 1mL/min, treats Deca
After the completion of, pH to 5.5 is adjusted with glacial acetic acid, after insulation reaction 17min, stand and be cooled to room temperature, subsequent sucking filtration simultaneously collects filter cake,
It is washed with deionized 4 times, at 47 DEG C, dries 22h, is prepared into modified Grafted Starch, standby；Count by weight, point
47 parts of 20% sodium chloride solutions of mass fraction of another name amount, the modified Grafted Starch of 12 parts of above-mentioned preparations, 2 parts of Hydrazoic acid,sodium salt and 7
Part soybean protein isolate is placed in conical flask, stirring mixing 27min, is evacuated to 12Pa and is placed in standing 22h, system at 2 DEG C
Standby mixed and modified liquid；By volume 1:1, normal hexane is mixed with the mixed and modified liquid stirring of above-mentioned preparation and is placed in beaker
In, subsequently to 5% sorbitan fatty ester of Deca normal hexane quality in beaker, stirring mixing is placed in high speed shear breast
In change machine, after emulsification pretreatment 12min, to adding the polyvinyl alcohol of normal hexane quality 3% in beaker, stirring mixing 4h at 47 DEG C,
Subsequent sucking filtration simultaneously collects filter cake, after being washed with deionized 4 times, dries 7h at 67 DEG C, is prepared into crosslinking tiny balloon；By weight
Amount number meter, weighs 27 parts of crosslinking tiny balloons, 32 parts of modified Grafted Starch and 12 parts of 5% tetraboric acids of mass fraction respectively
Sodium solution is placed in beaker, during stirring mixes and pours to mould, at room temperature, mould is placed in compacting 47s under 27MPa, with
Stand solidification 7h afterwards, then 7h is dried at 67 DEG C, be prepared into a kind of water soluble core-mould material by naturally cooling to room temperature.
Example 3
First in mass ratio 1:5, corn starch is mixed with the stirring of 1% sodium hydroxide solution of mass fraction, water-bath at 40 DEG C adds
Hot 30min, subsequently the acrylonitrile monemer of insulation Deca sodium hydroxide quality 30%, controls rate of addition for 1mL/min, treats Deca
After the completion of, pH to 5.5 is adjusted with glacial acetic acid, after insulation reaction 20min, stand and be cooled to room temperature, subsequent sucking filtration simultaneously collects filter cake,
It is washed with deionized 5 times, at 50 DEG C, dries 24h, is prepared into modified Grafted Starch, standby；Count by weight, point
50 parts of 20% sodium chloride solutions of mass fraction of another name amount, the modified Grafted Starch of 15 parts of above-mentioned preparations, 2 parts of Hydrazoic acid,sodium salt and
10 parts of soybean protein isolates are placed in conical flask, stirring mixing 30min, are evacuated to 15Pa and are placed in standing 24h at 5 DEG C,
It is prepared into mixed and modified liquid；By volume 1:1, normal hexane is mixed with the mixed and modified liquid stirring of above-mentioned preparation and is placed in beaker
In, subsequently to 5% sorbitan fatty ester of Deca normal hexane quality in beaker, stirring mixing is placed in high speed shear breast
In change machine, after emulsification pretreatment 15min, to adding the polyvinyl alcohol of normal hexane quality 3% in beaker, stirring mixing 5h at 50 DEG C,
Subsequent sucking filtration simultaneously collects filter cake, after being washed with deionized 5 times, dries 8h at 70 DEG C, is prepared into crosslinking tiny balloon；By weight
Amount number meter, weighs 30 parts of crosslinking tiny balloons, 35 parts of modified Grafted Starch and 15 parts of 5% tetraboric acids of mass fraction respectively
Sodium solution is placed in beaker, during stirring mixes and pours to mould, at room temperature, mould is placed in compacting 60s under 30MPa, with
Stand solidification 8h afterwards, then 8h is dried at 70 DEG C, be prepared into a kind of water soluble core-mould material by naturally cooling to room temperature.
Claims (1)
1. a kind of preparation method of water soluble core-mould material, it is characterised in that concrete preparation process is：
（1）In mass ratio 1:5, corn starch is mixed with the stirring of 1% sodium hydroxide solution of mass fraction, water at 35～40 DEG C
Bath 25～30min of heating, subsequently the acrylonitrile monemer of insulation Deca sodium hydroxide quality 30%, controls rate of addition for 1mL/
Min, after being added dropwise to complete, adjusts pH to 5.5 with glacial acetic acid, after 15～20min of insulation reaction, stands and is cooled to room temperature, subsequently
Sucking filtration simultaneously collects filter cake, is washed with deionized 3～5 times, at 45～50 DEG C dries 20～24h, is prepared into modified grafting beautiful
Rice starch, standby；
（2）Count by weight, weigh 45～50 parts of 20% sodium chloride solutions of mass fraction, 10～15 parts of above-mentioned preparations respectively
Modified Grafted Starch, 1～2 part of Hydrazoic acid,sodium salt and 5～10 parts of soybean protein isolates are placed in conical flask, stirring mixing 25
～30min, is evacuated to 10～15Pa and is placed in standing 20～24h at 0～5 DEG C, be prepared into mixed and modified liquid；
（3）By volume 1:1, normal hexane is mixed with the mixed and modified liquid stirring of above-mentioned preparation and is placed in beaker, subsequently right
5% sorbitan fatty ester of Deca normal hexane quality in beaker, stirring mixing are placed in high-speed shearing emulsion machine, are cut
After cutting 10～15min of emulsifying, to adding the polyvinyl alcohol of normal hexane quality 3% in beaker, at 45～50 DEG C stirring mixing 3～
5h, subsequent sucking filtration simultaneously collect filter cake, after being washed with deionized 3～5 times, dry 6～8h, be prepared into crosslinking at 65～70 DEG C
Tiny balloon；
（4）Count by weight, weigh 25～30 parts of crosslinking tiny balloons, 30～35 parts of steps respectively（1）Standby modification connects
Branch corn starch and 10～15 parts of 5% sodium tetraborate solution of mass fraction are placed in beaker, during stirring mixes and pours to mould,
At room temperature, mould is placed in 45～60s of compacting under 25～30MPa, subsequently stands 6～8h of solidification, then do at 65～70 DEG C
Dry 6～8h, is prepared into a kind of water soluble core-mould material by naturally cooling to room temperature.
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| CN201610870358.9A CN106496908A (en) | 2016-10-07 | 2016-10-07 | A kind of preparation method of water soluble core-mould material |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107674358A (en) * | 2017-10-23 | 2018-02-09 | 成都航空职业技术学院 | A kind of water soluble core-mould material and preparation method thereof |
| CN109181014A (en) * | 2018-08-17 | 2019-01-11 | 佛山朝鸿新材料科技有限公司 | A kind of preparation method of the aqueous core model material of high-strength stable |
| CN112646301A (en) * | 2020-12-24 | 2021-04-13 | 内蒙古航天红岗机械有限公司 | Preparation method of thermosetting resin compound reinforced water-soluble core mold |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107674358A (en) * | 2017-10-23 | 2018-02-09 | 成都航空职业技术学院 | A kind of water soluble core-mould material and preparation method thereof |
| CN109181014A (en) * | 2018-08-17 | 2019-01-11 | 佛山朝鸿新材料科技有限公司 | A kind of preparation method of the aqueous core model material of high-strength stable |
| CN112646301A (en) * | 2020-12-24 | 2021-04-13 | 内蒙古航天红岗机械有限公司 | Preparation method of thermosetting resin compound reinforced water-soluble core mold |
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Application publication date: 20170315 |