CN104479154A - Preparation method of completely biodegraded thin film - Google Patents
Preparation method of completely biodegraded thin film Download PDFInfo
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- CN104479154A CN104479154A CN201410777469.6A CN201410777469A CN104479154A CN 104479154 A CN104479154 A CN 104479154A CN 201410777469 A CN201410777469 A CN 201410777469A CN 104479154 A CN104479154 A CN 104479154A
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Abstract
The invention discloses a preparation method of a completely biodegraded thin film. The preparation method comprises the following steps: (1) mixing high amylosestarch with water to obtain starch milk with mass concentration of 13-17%, adjusting the pH value of the starch milk to 8.5-9.5 by 0.3-0.5mol/L sodium hydroxide, heating the starch milk to 90-110DEG C and gelatinizing for 20-40min at a stirring speed of 300-400r/min; (2) blending a polyvinyl alcohol water solution with mass concentration of 7-9% with the starch milk at a stirring speed of 100-140DEG C, wherein the mass ratio of the polyvinyl alcohol to the high amylose starch is 4: 6. The amylose starch content of the used high amylose maize starch is 80-82%; a glyoxal water solution is dripped to ensure that glyoxal is fully reacted to completely join the crosslinking; membrane liquid vacuum degassing is carried out to remove the bubbles caused in the stirring process.
Description
Technical field
The present invention relates to plastics film and manufacture field, particularly relate to a kind of preparation method of film of complete biodegradable.
Background technology
Plastics are since last century comes out, because it has the features such as proportion is little, production technique is simple, product category is various, both artistic and practical, penetrated into the every field such as industry, agricultural, national defence and daily life, by volume calculated, plastics have become output and the maximum material of consumption.While plastics are widely used, the problem existing for it also manifests day by day.On the one hand due to plastics stable performance, generally can not die away at short notice, and recovery difficult is large because plastic prod uses afterwards, processing cost is high, waste accumulating rate is fast, become the major reason of contaminate environment, serious threat, to the mankind and vegeto-animal living environment, becomes worldwide public hazards day by day.On the other hand, the raw material sources of most plastic prod is in petrochemical complex, and oil is a kind of Nonrenewable resources.Therefore, be especially that the biodegradable plastic of raw material has become the hot fields of competitively researching and developing countries in the world with starch with natural polymer.
The research of China to degradable plastic film is started in the photodegradable plastics film of 20 century 70s, and the emphasis of research and development is photodegradation, calcium carbonate-filled photodegradation and starch-filled plastic film, but the said products all can not be degradable.At present the developing focus of degradation plastic film is shifted to full biodegradation plastic film field.
Summary of the invention
The object of the invention is to solve current plastics film can not the problem of complete biodegradable, and provides a kind of preparation method of high amylose starches base thin film of complete biodegradable.
A kind of preparation method of film of complete biodegradable is prepared as follows:
(1) be the starch milk of 13% ~ 17% by high amylose starch water furnishing mass concentration, pH value of starch milk is regulated to be 8.5 ~ 9.5 with the sodium hydroxide of 0.3 ~ 0.5mol/L again, then starch milk is heated to 90 DEG C ~ 110 DEG C, gelatinization 20 ~ 40min under the stirring velocity of 300 ~ 400r/min;
(2) be the polyvinyl alcohol water solution of 7% ~ 9% by mass concentration, blended with starch milk under 100 ~ 140r/min stirring velocity, wherein the mass ratio of polyvinyl alcohol and high amylose starch is 4: 6;
(3) aqueous glycerin solution that mass concentration is 15 ~ 30% is added again, plasticizing reaction 20 ~ 40min under the condition of 100 ~ 105 DEG C, qualities of glycerin is 20% of starch and polyvinyl alcohol gross weight, then 85 DEG C ~ 90 DEG C are cooled the temperature to, be 2 ~ 5 by the pH value of the hydrochloric acid regulation system of 0.5 ~ 1mol/L, drip oxalic dialdehyde crosslinking reaction 30 ~ 50min, oxalic dialdehyde quality is 10% of starch and polyvinyl alcohol gross weight, add the water tolerance auxiliary agent urea reaction 15 ~ 25min of 2% of starch and polyvinyl alcohol gross weight, form film liquid;
(4) by film liquid vacuum outgas 10 ~ 20min, vacuum tightness is 0.06 ~ 0.09MPa, then by film liquid curtain coating in synthetic glass mould, under the condition of 60 DEG C ~ 80 DEG C, takes off film after dry 3 ~ 5 hours; Namely the high amylose starches base thin film of complete biodegradable is obtained.
Beneficial effect of the present invention
The amylose content of amylomaize of the present invention is 80% ~ 82%.Dripping glyoxal water solution is to allow oxalic dialdehyde fully react, and participate in crosslinked completely, the vacuum outgas of film liquid is to remove the bubble introduced in whipping process.
The product that the present invention produces, through scanning electron microscopic observation, section structure densification also has space net structure; Through X-ray diffraction analysis, there is certain crystalline texture; Analyze its thermal characteristics through differential scanning calorimeter to stablize, can normally use at 50 DEG C; Through Infrared spectroscopy, linking agent oxalic dialdehyde has participated in crosslinking reaction and remaining without surplus completely, monomer auxiliary agent can not occur in use and separate out.Simultaneously other auxiliary agents of the present invention are nontoxic and can the material of complete biodegradable, therefore have when product uses as various wrapping material free from environmental pollution, safety non-toxic, can be degradable etc. feature, its use properties has reached conventional polyolefins plastics film and apparently higher than common starch base degradable film, its biodegradability is obviously better than the environmental protection type packing material used in current large supermarket.The various performances measuring product are as follows: tensile strength 32.8MPa, elongation at break 135%, transmittance 42.1%, water-intake rate 41.7%, oil absorbency 0%, under normal temperature, soil pH value are the condition of 7.5 ~ 8.5 degrade 50 days time rate of weight loss can reach 68.2%, within 70 ~ 90 days, energy is degradable.The present invention has widened the raw material range preparing complete biodegradable film, and product has excellent use properties and degradation property.
Embodiment
Embodiment 1:
The high amylose starches base thin film of a kind of complete biodegradable of present embodiment is prepared as follows:
(1) be the starch milk of 13% by high amylose starch water furnishing mass concentration, then regulate pH value of starch milk to be 8.5 with the sodium hydroxide of 0.3mol/L, then starch milk is heated to 90 DEG C, gelatinization 20min under the stirring velocity of 300r/min;
(2) be the polyvinyl alcohol water solution of 7% by mass concentration, blended with starch milk under 100r/min stirring velocity, wherein the mass ratio of polyvinyl alcohol and high amylose starch is 4: 6;
(3) aqueous glycerin solution that mass concentration is 15% is added again, plasticizing reaction 20min under the condition of 100 DEG C, qualities of glycerin is 20% of starch and polyvinyl alcohol gross weight, then 85 DEG C are cooled the temperature to, be 2 by the pH value of the hydrochloric acid regulation system of 0.5mol/L, drip oxalic dialdehyde crosslinking reaction 30min, oxalic dialdehyde quality is 10% of starch and polyvinyl alcohol gross weight, add the water tolerance auxiliary agent urea reaction 15min of 2% of starch and polyvinyl alcohol gross weight, form film liquid;
(4) by film liquid vacuum outgas 10 ~ 20min, vacuum tightness is 0.06MPa, then by film liquid curtain coating in synthetic glass mould, under the condition of 60 DEG C, takes off film after dry 3 hours; Namely the high amylose starches base thin film of complete biodegradable is obtained.
Embodiment 2:
The high amylose starches base thin film of a kind of complete biodegradable of present embodiment is prepared as follows:
(1) be the starch milk of 17% by high amylose starch water furnishing mass concentration, then regulate pH value of starch milk to be 9.5 with the sodium hydroxide of 0.5mol/L, then starch milk is heated to 110 DEG C, gelatinization 40min under the stirring velocity of 400r/min;
(2) be the polyvinyl alcohol water solution of 9% by mass concentration, blended with starch milk under 140r/min stirring velocity, wherein the mass ratio of polyvinyl alcohol and high amylose starch is 5: 5;
(3) aqueous glycerin solution that mass concentration is 30% is added again, plasticizing reaction 40min under the condition of 105 DEG C, qualities of glycerin is 20% of starch and polyvinyl alcohol gross weight, then 90 DEG C are cooled the temperature to, be 5 by the pH value of the hydrochloric acid regulation system of 1mol/L, drip oxalic dialdehyde crosslinking reaction 50min, oxalic dialdehyde quality is 10% of starch and polyvinyl alcohol gross weight, add the water tolerance auxiliary agent urea reaction 25min of 2% of starch and polyvinyl alcohol gross weight, form film liquid;
(4) by film liquid vacuum outgas 20min, vacuum tightness is 0.09MPa, then by film liquid curtain coating in synthetic glass mould, under the condition of 80 DEG C, takes off film after dry 5 hours; Namely the high amylose starches base thin film of complete biodegradable is obtained.
Embodiment 3
The high amylose starches base thin film of a kind of complete biodegradable of present embodiment is prepared as follows:
(1) be the starch milk of 15% by high amylose starch water furnishing mass concentration, then regulate pH value of starch milk to be 9.0 with the sodium hydroxide of 0.4mol/L, then starch milk is heated to 100 DEG C, gelatinization 30min under the stirring velocity of 350r/min;
(2) be the polyvinyl alcohol water solution of 8% by mass concentration, blended with starch milk under 120r/min stirring velocity, wherein the mass ratio of polyvinyl alcohol and high amylose starch is 6: 4;
(3) aqueous glycerin solution that mass concentration is 22.5% is added again, plasticizing reaction 30min under the condition of 102.5 DEG C, qualities of glycerin is 20% of starch and polyvinyl alcohol gross weight, then 87.5 DEG C are cooled the temperature to, be 3.5 by the pH value of the hydrochloric acid regulation system of 0.75mol/L, drip oxalic dialdehyde crosslinking reaction 40min, oxalic dialdehyde quality is 10% of starch and polyvinyl alcohol gross weight, add the water tolerance auxiliary agent urea reaction 20min of 2% of starch and polyvinyl alcohol gross weight, form film liquid;
(4) by film liquid vacuum outgas 15min, vacuum tightness is 0.075MPa, then by film liquid curtain coating in synthetic glass mould, under the condition of 70 DEG C, takes off film after dry 4 hours; Namely the high amylose starches base thin film of complete biodegradable is obtained.
Claims (1)
1. a preparation method for the film of complete biodegradable, is characterized in that: be prepared as follows:
(1) be the starch milk of 13% ~ 17% by high amylose starch water furnishing mass concentration, pH value of starch milk is regulated to be 8.5 ~ 9.5 with the sodium hydroxide of 0.3 ~ 0.5mol/L again, then starch milk is heated to 90 DEG C ~ 110 DEG C, gelatinization 20 ~ 40min under the stirring velocity of 300 ~ 400r/min;
(2) be the polyvinyl alcohol water solution of 7% ~ 9% by mass concentration, blended with starch milk under 100 ~ 140r/min stirring velocity, wherein the mass ratio of polyvinyl alcohol and high amylose starch is 4: 6;
(3) aqueous glycerin solution that mass concentration is 15 ~ 30% is added again, plasticizing reaction 20 ~ 40min under the condition of 100 ~ 105 DEG C, qualities of glycerin is 20% of starch and polyvinyl alcohol gross weight, then 85 DEG C ~ 90 DEG C are cooled the temperature to, be 2 ~ 5 by the pH value of the hydrochloric acid regulation system of 0.5 ~ 1mol/L, drip oxalic dialdehyde crosslinking reaction 30 ~ 50min, oxalic dialdehyde quality is 10% of starch and polyvinyl alcohol gross weight, add the water tolerance auxiliary agent urea reaction 15 ~ 25min of 2% of starch and polyvinyl alcohol gross weight, form film liquid;
(4) by film liquid vacuum outgas 10 ~ 20min, vacuum tightness is 0.06 ~ 0.09MPa, then by film liquid curtain coating in synthetic glass mould, under the condition of 60 DEG C ~ 80 DEG C, takes off film after dry 3 ~ 5 hours; Namely the high amylose starches base thin film of complete biodegradable is obtained.
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| CN201410777469.6A CN104479154A (en) | 2014-12-16 | 2014-12-16 | Preparation method of completely biodegraded thin film |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106317470A (en) * | 2015-06-19 | 2017-01-11 | 大连瑞贤达塑胶有限公司 | Method for preparing high-strength starch-based completely biodegraded plastic film by solution blending method |
| CN108129701A (en) * | 2018-01-26 | 2018-06-08 | 上海理工大学 | A kind of method using big wheat husk production high performance plastic film |
| CN112940311A (en) * | 2021-02-02 | 2021-06-11 | 山东理工大学 | Preparation method of cross-linked modified film based on corn starch |
| CN113583368A (en) * | 2021-08-16 | 2021-11-02 | 安徽鼎洋生物基材料有限公司 | Modified starch PVA (polyvinyl alcohol) -based composite film and preparation method thereof |
-
2014
- 2014-12-16 CN CN201410777469.6A patent/CN104479154A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106317470A (en) * | 2015-06-19 | 2017-01-11 | 大连瑞贤达塑胶有限公司 | Method for preparing high-strength starch-based completely biodegraded plastic film by solution blending method |
| CN108129701A (en) * | 2018-01-26 | 2018-06-08 | 上海理工大学 | A kind of method using big wheat husk production high performance plastic film |
| CN112940311A (en) * | 2021-02-02 | 2021-06-11 | 山东理工大学 | Preparation method of cross-linked modified film based on corn starch |
| CN113583368A (en) * | 2021-08-16 | 2021-11-02 | 安徽鼎洋生物基材料有限公司 | Modified starch PVA (polyvinyl alcohol) -based composite film and preparation method thereof |
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