CN107628758A - A kind of preparation method of modified starch type glass fiber infiltration agent - Google Patents
A kind of preparation method of modified starch type glass fiber infiltration agent Download PDFInfo
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- CN107628758A CN107628758A CN201710804060.2A CN201710804060A CN107628758A CN 107628758 A CN107628758 A CN 107628758A CN 201710804060 A CN201710804060 A CN 201710804060A CN 107628758 A CN107628758 A CN 107628758A
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- starch
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- glass fiber
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- quartz sand
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Abstract
The invention discloses a kind of preparation method of modified starch type glass fiber infiltration agent, belong to glass fibre production field.The present invention is digested with isoamylase to buckwheat starch first,Etherification reaction is carried out again,Film forming agent is used as using modified starch,Viscosity strengthens,Cohesiveness degree is also improved,Add auxiliary film former,Improve and bond collection beam force,Modified starch and amylose are mixed,Film forming agent is improved to the decentralization of glass fibre and the intensity of glass fibre,Quartz sand is modified with silane coupler again,Plant oil decomposition is produced into lipophile ester group using microorganism,And in the self-crosslinking of microorganism,Enhance the compatibility of quartz sand and high polymer and improve its dispersed intensity,Also improve adhesion strength of the film forming agent to glass fibre,Add appropriate emulsifying agent,Surface tension can effectively be reduced,Size is set to be easier to soak fiberglass surfacing,Strengthen the mechanical strength and caking property of modified starch type glass fiber infiltration agent.
Description
Technical field
The invention discloses a kind of preparation method of modified starch type glass fiber infiltration agent, belongs to glass fibre production neck
Domain.
Background technology
Glass fiber textile is widely used in petrochemical industry, building decoration, adiabatic heat-insulation field.It is unprocessed
Glass fibre it is highly brittle, often need surface coating size to improve its performance.Different sizes can assign glass fibers
Different performances is tieed up, non-twist coarse sand, which must possess excellent textile performance, can just meet the needs of different product, Weave type leaching
Profit agent can not only improve the textile of glass, and can increase the intensity of glass-fiber-fabric.Size raw material and formula technique are systems
Make the key element of the most critical of the glass of high quality, and the link that glass production process is essential.In industry by it visually
It is compared to " chip fabrication techniques ".
Domestic many small and middle size fiberglass producers do not possess research and development, the ability of debugging infiltration agent prescription, ancient paraffin wax type also
Size, 711 sizes, 811 sizes are still using so that glass fiber product quality carries to come up, let alone produce multi items,
The glass fiber product of high profit, small lot.
At present, size film forming agent has five major classes：Epoxy, polyester, PVAC, acrylate and polyurethane.And epoxy emulsion
After film forming agent is most common and performance is a kind of well, but existing size using it in the presence of glass fibre is handled, glass fibers
Tie up the problem of composite material interface shear strength is not high.
Because the shortage of resource and the energy, the environmental pollution increasingly in expansion, and the earth of population have become the whole mankind
Anxious concern is needed, various countries are while the facility that modern science and technology is brought is enjoyed, it should also be appreciated that the mankind are i.e. by face
The extremely urgent environmental crisis faced.Therefore Green Chemistry becomes the major impetus of current international chemistry and chemical engineering science innovation
Source, Green Chemistry are the scientific methods for realizing that pollution prevention is most basic, have extremely important society and economic implications.
The content of the invention
The technical problems to be solved by the invention：For current size after glass fibre is handled using it, glass fibers
A kind of the defects of tieing up low composite material interface shear strength and film forming and poor caking property, there is provided modified starch type glass
The preparation method of fiber size.
In order to solve the above technical problems, the present invention is using technical scheme as described below：
A kind of preparation method of modified starch type glass fiber infiltration agent, it is characterised in that specifically preparation process is：
（1）30~50g buckwheat starch is weighed, 100~120mL water is added into buckwheat starch and is mixed, is formed sediment after stirring
Paste mixing liquid, gelatinized corn starch liquid is cooled down, with mass fraction be 1% salt acid for adjusting pH to 5~6, obtain starch mixed liquor, then to starch
3~6g isoamylases enzymolysis is added in mixed liquor, enzymolysis is filtered off except filter residue after terminating, and it is starch reaction liquid to obtain filtrate；
（2）The metabisulfite solution, 10~18mL mass point that 25~35mL mass fractions are 5% are added into starch reaction liquid successively
Number is that the expoxy propane that 2% sodium hydroxide solution and 20~30mL mass fractions are 0.5% mixes, after stirring reaction
To gelatinized starch suspension, continue, by gelatinized starch suspension and absolute ethyl alcohol mixing, to filter to obtain solid again after stirring
Thing, continue to grind solids, obtain modified starch；
（3）The crushing of 60~80g quartzite sand grinds is weighed again, quartz sand powder is obtained, by quartz sand powder and silane coupler
KH792 is mixed, and obtains mixture, continues to add the rapeseed oil and mixture quality of mixture quality 7% into mixture
0.7% Grape Skin, is fitted into fermentation tank, is sealed by fermentation, and after fermentation ends, takes out tunning, as Modified Quartz Sand powder
End；
（4）Count in parts by weight, weigh modified starch, buckwheat starch, water, Modified Quartz Sand powder mixed liquor respectively and be placed in stirring
It is stirred in machine, then adds peanut oil, gelatin and polyoxyethanyl ester, continues to be stirred, drying is cooled to room temperature, discharges,
It can be prepared by modified starch type glass fiber infiltration agent.
Step（1）Described whipping temp is 85~105 DEG C, and mixing time is 1~2h, and cool time is 40~50 DEG C,
Hydrolysis temperature is 25~35 DEG C, and enzymolysis time is 1~2h.
Step（2）Described whipping temp is 25~45 DEG C, and mixing time be 20~30min, gelatinized starch suspension with
The volume ratio of ethanol is 3：1, continuation mixing time is 10~15min, and milling time is 6~10min.
Step（3）Described milling time is 8~10min, and quartz sand powder and silane coupler KH792 mass ratio are
8：1, mixing time is 15~20min, and fermentation temperature is 35~45 DEG C, and fermentation time is 6~8 days.
Step（4）Described meter in parts by weight, weigh respectively 20~40 portions of modified starches, 10~30 parts of buckwheat starch,
60~80 parts of water, 10~12 parts of Modified Quartz Sand powder, 3~5 portions of peanut oil, 2~4 parts of gelatin and 1~3 part of polyoxyethanyl ester,
Whipping temp is 30~50 DEG C, and mixing time be 15~24min, and it is 55~75 DEG C to continue whipping temp, mixing time for 20~
30min。
The beneficial effects of the invention are as follows：
The present invention is digested with isoamylase to buckwheat starch first, then is carried out etherification reaction, produces modified starch, with
Modified starch is as film forming agent, and because the viscosity of modified starch strengthens, therefore film forming agent is to the cohesiveness journey of fiberglass surfacing
Degree is also improved, and adds auxiliary film former, is further improved size and is bonded collection beam force, and buckwheat starch is amylose,
Modified starch and amylose are mixed, improve film forming agent again to the decentralization of glass fibre and the intensity of glass fibre,
Quartz sand is modified with silane coupler again, by itself and vegetable oil and Grape Skin blending fermentation, using microorganism by vegetable oil
Decompose and produce lipophile ester group, and cause ester group to be grafted to segment glass fiber surface under the self-crosslinking of microorganism, increase
The compatibility of strong quartz sand and high polymer and improve its dispersed intensity, also improve film forming agent and glass fibre is glued
Knotting strength, appropriate emulsifying agent is continuously added, can effectively reduce the surface tension of sizing system, make size be easier to moisten
Wet glass fiber surface, further enhance the mechanical strength and caking property of modified starch type glass fiber infiltration agent.
Embodiment
30~50g buckwheat starch is weighed, 100~120mL water is added into buckwheat starch, mixes and stirs at 85~105 DEG C
1~2h is mixed, gelatinized corn starch liquid is obtained after stirring, gelatinized corn starch liquid is cooled to 40~50 DEG C, is 1% salt acid for adjusting pH with mass fraction
To 5~6, starch mixed liquor is obtained, then adds 3~6g isoamylases into starch mixed liquor and 1~2h is digested at 25~35 DEG C,
Enzymolysis is filtered off except filter residue after terminating, and it is starch reaction liquid to obtain filtrate, adds 25~35mL into starch reaction liquid successively
The sodium hydroxide solution and 20~30mL mass point that metabisulfite solution that mass fraction is 5%, 10~18mL mass fractions are 2%
Number is 0.5% expoxy propane, and 20~30min is mixed at 25~45 DEG C, and it is suspended to obtain gelatinized starch after stirring reaction
Liquid, it is by volume 3：Gelatinized starch suspension and absolute ethyl alcohol are mixed 10~15min by 1, filter to obtain again after stirring
Solids, continue by solids grind 6~10min, obtain modified starch, then weigh 60~80g quartzite sand grinds crush 8~
10min, quartz sand powder is obtained, be in mass ratio 8：1 quartz sand powder and silane coupler KH792 mixed 15~
20min, mixture is obtained, continue to add the rapeseed oil of mixture quality 7% and the grape of mixture quality 0.7% into mixture
Skin, it is fitted into fermentation tank, is sealed by fermentation 6~8 days under conditions of being 35~45 DEG C in temperature, after fermentation ends, takes out fermentation production
Thing, as Modified Quartz Sand powder, are counted in parts by weight, weigh respectively 20~40 portions of modified starches, 10~30 parts of buckwheat starch,
60~80 parts of water, 10~12 portions of Modified Quartz Sand powder mixed liquors are placed in mixer, it is stirred 15 at 30~50 DEG C~
24min, then 3~5 portions of peanut oil, 2~4 parts of gelatin and 1~3 part of polyoxyethanyl ester are added, continue to stir at 55~75 DEG C and mix
20~30min is closed, drying is cooled to room temperature, discharges, you can modified starch type glass fiber infiltration agent is made.
Example 1
30g buckwheat starch is weighed, 100mL water is added into buckwheat starch, 1h is mixed at 85 DEG C, starch is obtained after stirring
Paste liquid, gelatinized corn starch liquid be cooled to 40 DEG C, with mass fraction be 1% salt acid for adjusting pH to 5, obtain starch mixed liquor, then to shallow lake
3g isoamylases are added in powder mixed liquor 1h is digested at 25 DEG C, enzymolysis is filtered off except filter residue after terminating, and it is to form sediment to obtain filtrate
Powder reaction solution, adding metabisulfite solution, 10mL mass fractions that 25mL mass fractions are 5% into starch reaction liquid successively is
2% sodium hydroxide solution and 20mL mass fractions is 0.5% expoxy propane, and 20min is mixed at 25 DEG C, and stirring is anti-
Should after obtain gelatinized starch suspension, be by volume 3：Gelatinized starch suspension and absolute ethyl alcohol are mixed 10min by 1,
Filter to obtain solids again after stirring, continue solids grinding 6min, obtain modified starch, then weigh 60g quartzite sand grinds
8min is crushed, quartz sand powder is obtained, is in mass ratio 8：1 mixes quartz sand powder and silane coupler KH792
15min, mixture is obtained, continue to add the rapeseed oil of mixture quality 7% and the grape of mixture quality 0.7% into mixture
Skin, it is fitted into fermentation tank, is sealed by fermentation 6 days under conditions of being 35 DEG C in temperature, after fermentation ends, takes out tunning, be
Modified Quartz Sand powder, is counted in parts by weight, weighs 20 portions of modified starches, 10 parts of buckwheat starch, 60 parts of water, 10 parts of modifications respectively
Quartz sand powder mixed liquor is placed in mixer, and 15min is stirred at 30 DEG C, then adds 3 portions of peanut oil, 2 parts of gelatin and 1
Part polyoxyethanyl ester, continues to be stirred 20min at 55 DEG C, and drying is cooled to room temperature, discharges, you can modified starch type is made
Glass fiber infiltration agent.
Example 2
40g buckwheat starch is weighed, 110mL water is added into buckwheat starch, 1h is mixed at 95 DEG C, starch is obtained after stirring
Paste liquid, gelatinized corn starch liquid be cooled to 45 DEG C, with mass fraction be 1% salt acid for adjusting pH to 5, obtain starch mixed liquor, then to shallow lake
4g isoamylases are added in powder mixed liquor 1h is digested at 30 DEG C, enzymolysis is filtered off except filter residue after terminating, and it is to form sediment to obtain filtrate
Powder reaction solution, adding metabisulfite solution, 15mL mass fractions that 30mL mass fractions are 5% into starch reaction liquid successively is
2% sodium hydroxide solution and 25mL mass fractions is 0.5% expoxy propane, and 25min is mixed at 30 DEG C, and stirring is anti-
Should after obtain gelatinized starch suspension, be by volume 3：Gelatinized starch suspension and absolute ethyl alcohol are mixed 12min by 1,
Filter to obtain solids again after stirring, continue solids grinding 8min, obtain modified starch, then weigh 70g quartzite sand grinds
9min is crushed, quartz sand powder is obtained, is in mass ratio 8：1 mixes quartz sand powder and silane coupler KH792
18min, mixture is obtained, continue to add the rapeseed oil of mixture quality 7% and the grape of mixture quality 0.7% into mixture
Skin, it is fitted into fermentation tank, is sealed by fermentation 7 days under conditions of being 40 DEG C in temperature, after fermentation ends, takes out tunning, be
Modified Quartz Sand powder, is counted in parts by weight, weighs 30 portions of modified starches, 20 parts of buckwheat starch, 70 parts of water, 11 parts of modifications respectively
Quartz sand powder mixed liquor is placed in mixer, and 20min is stirred at 40 DEG C, then adds 4 portions of peanut oil, 3 parts of gelatin and 2
Part polyoxyethanyl ester, continues to be stirred 25min at 60 DEG C, and drying is cooled to room temperature, discharges, you can modified starch type is made
Glass fiber infiltration agent.
Example 3
50g buckwheat starch is weighed, 120mL water is added into buckwheat starch, 2h is mixed at 105 DEG C, is formed sediment after stirring
Paste mixing liquid, gelatinized corn starch liquid is cooled to 50 DEG C, with mass fraction be 1% salt acid for adjusting pH to 6, obtain starch mixed liquor, then to
6g isoamylases are added in starch mixed liquor 2h is digested at 35 DEG C, enzymolysis is filtered off except filter residue after terminating, and obtaining filtrate is
Starch reaction liquid, adding metabisulfite solution, 18mL mass fractions that 35mL mass fractions are 5% into starch reaction liquid successively is
2% sodium hydroxide solution and 30mL mass fractions is 0.5% expoxy propane, and 30min is mixed at 45 DEG C, and stirring is anti-
Should after obtain gelatinized starch suspension, be by volume 3：Gelatinized starch suspension and absolute ethyl alcohol are mixed 15min by 1,
Filter to obtain solids again after stirring, continue solids grinding 10min, obtain modified starch, then weigh 80g quartzite sand grinds
10min is crushed, quartz sand powder is obtained, is in mass ratio 8：1 mixes quartz sand powder and silane coupler KH792
20min, mixture is obtained, continue to add the rapeseed oil of mixture quality 7% and the grape of mixture quality 0.7% into mixture
Skin, it is fitted into fermentation tank, is sealed by fermentation 8 days under conditions of being 45 DEG C in temperature, after fermentation ends, takes out tunning, be
Modified Quartz Sand powder, is counted in parts by weight, weighs 40 portions of modified starches, 30 parts of buckwheat starch, 80 parts of water, 12 parts of modifications respectively
Quartz sand powder mixed liquor is placed in mixer, and 24min is stirred at 50 DEG C, then adds 5 portions of peanut oil, 4 parts of gelatin and 3
Part polyoxyethanyl ester, continues to be stirred 30min at 75 DEG C, and drying is cooled to room temperature, discharges, you can modified starch type is made
Glass fiber infiltration agent.
The size that comparative example is produced with Wuxi City company is as a comparison case to modified starch type produced by the present invention
Size in glass fiber infiltration agent and comparative example is detected, and testing result is as shown in table 1：1st, method of testing
Stiffness test is detected by GB/T7690.4 regulation.
Adhesion strength test is detected by JG/T298-2010 regulation.
Impregnability test is detected by GB21352-2008 regulation.
Table 1
It can be seen from data in table 1, the stiffness of modified starch type glass fiber infiltration agent produced by the present invention is low, film forming
It is good, and adhesion strength is big, has wide prospect of the application.
Claims (5)
1. a kind of preparation method of modified starch type glass fiber infiltration agent, it is characterised in that specifically preparation process is：
（1）30~50g buckwheat starch is weighed, 100~120mL water is added into buckwheat starch and is mixed, is formed sediment after stirring
Paste mixing liquid, gelatinized corn starch liquid is cooled down, with mass fraction be 1% salt acid for adjusting pH to 5~6, obtain starch mixed liquor, then to starch
3~6g isoamylases enzymolysis is added in mixed liquor, enzymolysis is filtered off except filter residue after terminating, and it is starch reaction liquid to obtain filtrate；
（2）The metabisulfite solution, 10~18mL mass that 25~35mL mass fractions are 5% are added into starch reaction liquid successively
The expoxy propane that the sodium hydroxide solution and 20~30mL mass fractions that fraction is 2% are 0.5% mixes, after stirring reaction
Gelatinized starch suspension is obtained, continues, by gelatinized starch suspension and absolute ethyl alcohol mixing, to filter and consolidated again after stirring
Body thing, continue to grind solids, obtain modified starch；
（3）The crushing of 60~80g quartzite sand grinds is weighed again, quartz sand powder is obtained, by quartz sand powder and silane coupler
KH792 is mixed, and obtains mixture, continues to add the rapeseed oil and mixture quality of mixture quality 7% into mixture
0.7% Grape Skin, is fitted into fermentation tank, is sealed by fermentation, and after fermentation ends, takes out tunning, as Modified Quartz Sand powder
End；
（4）Count in parts by weight, weigh modified starch, buckwheat starch, water, Modified Quartz Sand powder mixed liquor respectively and be placed in stirring
It is stirred in machine, then adds peanut oil, gelatin and polyoxyethanyl ester, continues to be stirred, drying is cooled to room temperature, discharges,
It can be prepared by modified starch type glass fiber infiltration agent.
A kind of 2. preparation method of modified starch type glass fiber infiltration agent according to claim 1, it is characterised in that：Step
Suddenly（1）Described whipping temp is 85~105 DEG C, and mixing time is 1~2 h, and cool time is 40~50 DEG C, hydrolysis temperature
For 25~35 DEG C, enzymolysis time is 1~2h.
A kind of 3. preparation method of modified starch type glass fiber infiltration agent according to claim 1, it is characterised in that：Step
Suddenly（2）Described whipping temp is 25~45 DEG C, and mixing time is 20~30min, gelatinized starch suspension and ethanol volume
Than for 3：1, continuation mixing time is 10~15min, and milling time is 6~10min.
A kind of 4. preparation method of modified starch type glass fiber infiltration agent according to claim 1, it is characterised in that：Step
Suddenly（3）Described milling time is 8~10min, and quartz sand powder and silane coupler KH792 mass ratio are 8：1, during stirring
Between be 15~20min, fermentation temperature is 35~45 DEG C, and fermentation time is 6~8 days.
A kind of 5. preparation method of modified starch type glass fiber infiltration agent according to claim 1, it is characterised in that：Step
Suddenly（4）Described meter in parts by weight, weigh respectively 20~40 portions of modified starches, 10~30 parts of buckwheat starch, 60~80 parts of water,
10~12 parts of Modified Quartz Sand powder, 3~5 portions of peanut oil, 2~4 parts of gelatin and 1~3 part of polyoxyethanyl ester, whipping temp 30
~50 DEG C, mixing time is 15~24min, and it is 55~75 DEG C to continue whipping temp, and mixing time is 20~30min.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108996925A (en) * | 2018-07-27 | 2018-12-14 | 苏州华龙化工有限公司 | A kind of preparation method of enhanced type glass fiber impregnating agent |
| CN110156346A (en) * | 2019-05-27 | 2019-08-23 | 泰安顺茂新材料技术有限公司 | A kind of Wrapping formed fiberglass surface modifiers and preparation method thereof |
| CN111977990A (en) * | 2020-09-08 | 2020-11-24 | 清远忠信电子材料有限公司 | High-performance impregnating compound for superfine electronic yarn and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103012608A (en) * | 2012-11-21 | 2013-04-03 | 西南科技大学 | Method for preparing etherification linear-chain dextrin starch film-forming agent for glass fiber infiltration |
| CN103121800A (en) * | 2013-03-06 | 2013-05-29 | 东华大学 | Impregnating compound added with inorganic nano particles for glass fiber |
| EP3135647A1 (en) * | 2015-08-28 | 2017-03-01 | Rockwool International A/S | Solid state binder |
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2017
- 2017-09-08 CN CN201710804060.2A patent/CN107628758A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103012608A (en) * | 2012-11-21 | 2013-04-03 | 西南科技大学 | Method for preparing etherification linear-chain dextrin starch film-forming agent for glass fiber infiltration |
| CN103121800A (en) * | 2013-03-06 | 2013-05-29 | 东华大学 | Impregnating compound added with inorganic nano particles for glass fiber |
| EP3135647A1 (en) * | 2015-08-28 | 2017-03-01 | Rockwool International A/S | Solid state binder |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108996925A (en) * | 2018-07-27 | 2018-12-14 | 苏州华龙化工有限公司 | A kind of preparation method of enhanced type glass fiber impregnating agent |
| CN110156346A (en) * | 2019-05-27 | 2019-08-23 | 泰安顺茂新材料技术有限公司 | A kind of Wrapping formed fiberglass surface modifiers and preparation method thereof |
| CN110156346B (en) * | 2019-05-27 | 2022-04-12 | 泰安顺茂新材料技术有限公司 | Winding forming glass fiber surface modifier and preparation method thereof |
| CN111977990A (en) * | 2020-09-08 | 2020-11-24 | 清远忠信电子材料有限公司 | High-performance impregnating compound for superfine electronic yarn and preparation method thereof |
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Effective date of registration: 20180417 Address after: 213000 Room 502, unit 54, Lihua three village, Tianning District, Changzhou, Jiangsu, China Applicant after: Zhou Rong Address before: 213164 B 2519, Beijing University of Chemical Technology Research Institute, Changzhou science and Education City, 801 Wujin Road, Wujin, Changzhou. Applicant before: TRUSYN CHEM-TECH CO., LTD. |
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