CN104530491A - Preparation method of amylocellulose composite material - Google Patents
Preparation method of amylocellulose composite material Download PDFInfo
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- CN104530491A CN104530491A CN201410769456.4A CN201410769456A CN104530491A CN 104530491 A CN104530491 A CN 104530491A CN 201410769456 A CN201410769456 A CN 201410769456A CN 104530491 A CN104530491 A CN 104530491A
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Abstract
The invention relates to a preparation method of an amylocellulose composite material. The preparation method comprises the following steps: dissolving modified starch and modified cellulose into water, uniformly mixing, and carrying out spray drying to obtain powder; adding a cross-linking agent to an organic solvent for cross-linking reaction; then filtering, washing and drying to obtain a product, wherein the cellulose is 5%-50%, and the modified starch is 50%-95%, the addition amount of the cross-linking agent accounts for 0.01%-0.1% of total amount of the cellulose and the modified starch, the modified starch can be dissolved in the water at 1-50 DEG C, the cross-linking agent is a chemical reagent capable of being reacted with the starch and cellulose hydroxy, the concentration of a feed liquid is 3%-20% during the spray drying, the air inlet temperature is 150-200 DEG C, and the air outlet temperature is 80-100 DEG C. The preparation method disclosed by the invention can be used for solving the problem of immiscibility of simple mixing of the cellulose and the starch and meets the requirements of different application fields by preparing ionic and nonionic composite materials.
Description
Technical field
The present invention relates to a kind of preparation method of matrix material, specifically relate to a kind of preparation method of farinose matrix material, obtained matrix material can be used as membrane-forming agent, tackiness agent, embedding medium, is applied to the field such as medicine, food.
Background technology
Modified cellulose, as the good material of one, is widely applied in fields such as medicine, food, chemical industry.But because modified cellulose is complicated in preparation method, cost is higher, such as apply capsule material prepared by HPMC, be more than 2 times of traditional gelatine capsule cost, therefore extravagent price limits the broader applications of Mierocrystalline cellulose in every field.Starch is same with Mierocrystalline cellulose comes from plant, wide material sources.Further, compared to Mierocrystalline cellulose, starch cost is lower.Starch on molecular structure to Mierocrystalline cellulose and similar, but starch differs comparatively large with cellulose character, starch is easily aging, age of starch reason is that between starch molecule bundle, hydroxyl forms hydrogen bond, make starch bundle form new crystallizing field, cause that starch material is hardening to become fragile.Preventing age of starch from having become the common problem of industry, is also a global difficult problem.Mierocrystalline cellulose is because be not easy between its structure to form hydrogen bond, so not easily aging, therefore as introduced modified cellulose in modified starch, form new material, this matrix material will have starch and cellulosic feature, can change the character of Mierocrystalline cellulose and starch simultaneously, prevent age of starch.This method can make novel material have cellulosic advantageous property, reduces costs simultaneously, the alternative Mierocrystalline cellulose of novel material.
In practical application, most of starch and Mierocrystalline cellulose are immiscible, as hydroxypropylated starch and Natvosol, when dissolving separately easily, but layering can occur after two kinds of solution mixing.Even if the bi-material dissolved each other, does not also influence each other between them, show character single separately.Therefore, patent of the present invention is proposed.
Summary of the invention
For the above-mentioned technical problem of prior art, the object of this invention is to provide a kind of preparation method of farinose matrix material, make modified starch become as a whole with modified cellulose by chemical process, make this matrix material have starch and cellulosic character simultaneously.This method solve simple cellulose mixture and the immiscible problem of starch, ionic and non-ionic type two kinds of matrix materials can be prepared, to meet the demand in different application field.
For achieving the above object, the present invention is achieved by the following technical solutions:
A preparation method for farinose matrix material, comprises the following steps: be dissolved in water by modified starch and modified cellulose, mix, spraying dry, obtains powder, adds linking agent in organic solvent and carries out crosslinking reaction, filter after reaction, washing, dry and obtain product;
By weight percentage, described Mierocrystalline cellulose is 5%-50%, and modified starch is 50%-95%;
Described linking agent add the 0.01%-1% that weight is Mierocrystalline cellulose and modified starch total amount;
Described modified starch is solubilized in 1-50 DEG C of water; Described linking agent is the chemical reagent that can react with starch and cellulose hydroxyl group;
Charging feed concentration during described spraying dry is 3-20%, and inlet temperature is 150-200 DEG C, and air outlet temperature is 80-100 DEG C.
As preferably, the temperature of described crosslinking reaction is 20-60 DEG C, and the reaction times is 1-20 hour.
As preferably, the organic solvent washing of described washing 80-95%, the temperature of described oven dry is 30-100 DEG C.
As preferably, described organic solvent can be methyl alcohol, ethanol or Virahol, and the concentration of organic solvent is 60-95%, and surplus is water.
Described modified starch is carboxymethyl starch, hydroxypropylated starch, starch Sodium Octenyl Succinate or pregelatinized Starch.
Described modified cellulose is carboxymethyl cellulose, hydroxypropylcellulose, Natvosol or HPMC.
Described linking agent is epoxy chloropropane or Trisodium trimetaphosphate.
Reaction equation of the present invention is as follows:
, wherein R is hydroxyl or denaturing group, and linking agent is epoxy chloropropane.
The preparation method of a kind of farinose matrix material of the present invention, modified starch and modified cellulose are dissolved in water, mix, and spraying dry obtains powder, carry out crosslinking reaction in organic solvent, filter after reaction, and washing is dried.The farinose matrix material prepared by the present invention overcomes starch and the immiscible problem of Mierocrystalline cellulose, and meanwhile, matrix material is provided with and individual fibers element difference characteristic, as solubility property.Novel material prepared by the present invention overcomes the easily aging shortcoming of starch, can be used for alternative fiber element, reduces costs.This composite material can be used for membrane-forming agent, tackiness agent or embedding medium.
Embodiment
Below in conjunction with specific embodiment, the present invention is further illustrated, but protection scope of the present invention is not limited to this.
The raw material related in the present invention all can be synthesized by mode well known in the art, also can adopt commercially available prod.
When R is that (denaturing group refers to: starch is carboxymethyl, hydroxypropyl or octenyl succinic acid groups for hydroxyl or denaturing group in the present invention; Mierocrystalline cellulose is carboxymethyl, hydroxypropyl, hydroxyethyl or hydroxypropylmethyl), when linking agent is epoxy chloropropane, reaction equation is as follows:
.
embodiment 1
The carboxymethyl starch of 95% and the carboxymethyl cellulose of 5% are dissolved in water, mix, feed concentration 3%, spraying dry inlet temperature 150 DEG C, air outlet temperature 80 DEG C, obtains powder, is dispersed in by powder in 80% concentration ethanol, temperature 60 C, take epoxy chloropropane as linking agent, add-on is 1%, crosslinking reaction 20 hours, filter after reaction, with 80% ethanolic soln washing, 30 DEG C of oven dry, obtained carboxymethyl starch cellulose composite material, this composite emulsion viscosities 10000mpas, can be applicable to tackiness agent.
embodiment 2
The hydroxypropylated starch of 50% and the Natvosol of 50% are dissolved in water, mix, feed concentration 5%, spraying dry inlet temperature 200 DEG C, air outlet temperature 100 DEG C, obtains powder, powder is dispersed in 60% concentration ethanol, temperature 50 C, take epoxy chloropropane as linking agent, add-on is 0.01%, crosslinking reaction 10 hours, filter after reaction, with 80% ethanolic soln washing, 50 DEG C of oven dry.Obtained hydroxypropylated starch Natvosol matrix material.
After this matrix material dissolves, solution forms a homogeneous phase.This material can be used for preparing capsule.
embodiment 3
By the starch Sodium Octenyl Succinate of 90% and the hydroxypropylcellulose of 10%, mix, feed concentration 20%, spraying dry inlet temperature 200 DEG C, air outlet temperature 100 DEG C, obtains powder, powder is dispersed in 95% concentration ethanol, temperature 60 C, take epoxy chloropropane as linking agent, add-on is 1%, crosslinking reaction 1 hour, filter after reaction, with 95% ethanolic soln washing, 100 DEG C of oven dry.Obtained farinose matrix material.This matrix material film-forming properties and stability are greatly improved, and can be applicable to powdery oil.
embodiment 4
By the pregelatinized Starch of 80% and the HPMC of 20%, mix, feed concentration 10%, spraying dry inlet temperature 180 DEG C, air outlet temperature 90 DEG C, obtains powder, powder is dispersed in 80% concentration ethanol, temperature 40 DEG C, take Trisodium trimetaphosphate as linking agent, add-on is 0.5%, crosslinking reaction 15 hours, filter after reaction, with 80% ethanolic soln washing, 50 DEG C of oven dry.Obtained farinose matrix material.This matrix material dissolving performance is identical with pregelatinized Starch.Can dissolve in 1-99 DEG C of water, Cheng Yixiang.
embodiment 5
By the pregelatinized Starch of 40% and the HPMC of 60%, mix, feed concentration 15%, spraying dry inlet temperature 175 DEG C, air outlet temperature 85 DEG C, obtains powder, powder is dispersed in 70% concentration methyl alcohol, temperature 30 DEG C, take Trisodium trimetaphosphate as linking agent, add-on is 0.6%, crosslinking reaction 5 hours, filter after reaction, with 95% methanol solution washing, 100 DEG C of oven dry.Obtained farinose matrix material.This matrix material dissolving performance is identical with pregelatinized Starch.Can dissolve in 1-99 DEG C of water, Cheng Yixiang.
embodiment 6
By the starch Sodium Octenyl Succinate of 90% and the hydroxypropylcellulose of 10%, mix, feed concentration 20%, spraying dry inlet temperature 200 DEG C, air outlet temperature 100 DEG C, obtains powder, powder is dispersed in 75% concentration Virahol, temperature 60 C, take Trisodium trimetaphosphate as linking agent, add-on is 1%, crosslinking reaction 1 hour, filter after reaction, with 95% aqueous isopropanol washing, 100 DEG C of oven dry.Obtained farinose matrix material.This matrix material film-forming properties and stability are greatly improved, and can be applicable to powdery oil.
The preparation method of a kind of farinose matrix material of the present invention, modified starch and modified cellulose are dissolved in water, mix, and spraying dry obtains powder, carry out crosslinking reaction in organic solvent, filter after reaction, and washing is dried.The farinose matrix material prepared by the present invention overcomes starch and the immiscible problem of Mierocrystalline cellulose, and meanwhile, matrix material is provided with and individual fibers element difference characteristic.Novel material prepared by the present invention overcomes the easily aging shortcoming of starch, can be used for alternative fiber element, reduces costs.This composite material can be used for membrane-forming agent, tackiness agent or embedding medium.
Above-described embodiment only illustrates inventive concept of the present invention for explaining, but not the restriction to rights protection of the present invention, all changes utilizing this design the present invention to be carried out to unsubstantiality, all should fall into protection scope of the present invention.
Claims (8)
1. the preparation method of a farinose matrix material, it is characterized in that comprising the following steps: modified starch and modified cellulose are dissolved in water, mix, spraying dry, obtain powder, add linking agent in organic solvent and carry out crosslinking reaction, filter after reaction, washing, dries and obtains product;
By weight percentage, described Mierocrystalline cellulose is 5%-50%, and modified starch is 50%-95%;
Described linking agent add the 0.01%-1% that weight is Mierocrystalline cellulose and modified starch total amount;
Described modified starch is solubilized in 1-50 DEG C of water; Described linking agent is the chemical reagent that can react with starch and cellulose hydroxyl group;
Charging feed concentration during described spraying dry is 3-20%, and inlet temperature is 150-200 DEG C, and air outlet temperature is 80-100 DEG C.
2. the preparation method of farinose matrix material as claimed in claim 1, is characterized in that: the temperature of described crosslinking reaction is 20-60 DEG C, and the reaction times is 1-20 hour.
3. the preparation method of farinose matrix material as claimed in claim 1, it is characterized in that: the organic solvent washing of described washing 80-95%, the temperature of described oven dry is 30-100 DEG C.
4. the preparation method of farinose matrix material as described in claim 1 or 3, it is characterized in that: described organic solvent can be methyl alcohol, ethanol or Virahol, the concentration of organic solvent is 60-95%, and surplus is water.
5. the preparation method of farinose matrix material as claimed in claim 1, is characterized in that: described modified starch is carboxymethyl starch, hydroxypropylated starch, starch Sodium Octenyl Succinate or pregelatinized Starch.
6. the preparation method of farinose matrix material as claimed in claim 1, is characterized in that: described modified cellulose is carboxymethyl cellulose, hydroxypropylcellulose, Natvosol or HPMC.
7. the preparation method of farinose matrix material as claimed in claim 1, is characterized in that: described linking agent is epoxy chloropropane or Trisodium trimetaphosphate.
8. the preparation method of farinose matrix material as claimed in claim 7, is characterized in that described reaction equation is as follows:
, wherein R is hydroxyl or denaturing group, and linking agent is epoxy chloropropane.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104888227A (en) * | 2015-05-26 | 2015-09-09 | 山东瑞元生物科技股份有限公司 | Hydroxypropyl starch copolymer for hollow capsules and preparation method of capsules taking hydroxypropyl starch copolymer as raw material |
| CN105914376A (en) * | 2016-06-24 | 2016-08-31 | 辽宁九夷锂能股份有限公司 | Reinforced type composite binder for negative electrode of lithium ion battery and application of reinforced type composite binder |
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| CN104888227A (en) * | 2015-05-26 | 2015-09-09 | 山东瑞元生物科技股份有限公司 | Hydroxypropyl starch copolymer for hollow capsules and preparation method of capsules taking hydroxypropyl starch copolymer as raw material |
| CN104888227B (en) * | 2015-05-26 | 2019-10-18 | 山东瑞元生物科技股份有限公司 | Capsules hydroxypropul starch copolymer and using the hydroxypropul starch copolymer as the preparation method of the capsule of raw material |
| CN105914376A (en) * | 2016-06-24 | 2016-08-31 | 辽宁九夷锂能股份有限公司 | Reinforced type composite binder for negative electrode of lithium ion battery and application of reinforced type composite binder |
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