A kind of starch sulfate and its salt synthesis process

Abstract

The invention relates to a kind of biomass raw material with starch as the main component and SO in an aprotic halogenated alkyl solvent 3 A new clean production process for synthesizing water-soluble starch sulfate with smooth reaction and high conversion rate. Utilizing the process can fully expand the use of starch-containing biomass raw materials, and the water solubility and binding performance of the product are significantly improved. The process is simple, the production process is clean and environmentally friendly, the conditions are mild, unreacted materials can be directly used or recycled, no toxic side ions and solvent residues, the product is light in color, safe and environmentally friendly, and can be used in a wide range of applications. It has huge industrial application prospects and significant The economic and ecological benefits meet the strategic requirements of vigorously developing natural renewable resources and sustainable development.

Description

technical field

[0001] The invention relates to a new synthesis process of starch sulfate and its salt, which belongs to the technical field of starch modification. Background technique

[0002] Starch is a high-molecular carbohydrate widely present in the roots, stems, seeds and other tissues of most plants. Amylose is mainly linked by D-glucopyranose via α-1,4 glycosidic bonds. It is a linear polymer; and amylopectin is a nonlinear polymer connected by α-1,4 glycosidic bonds and α-1,6 glycosidic bonds. There is an alcoholic hydroxyl group at the 2, 3, and 6 positions of each anhydroglucose unit in the starch molecule, and the primary hydroxyl group at the 6-position carbon atom has the highest activity, followed by the secondary hydroxyl groups at the 2nd and 3rd positions.

[0003] Although starch molecules are rich in hydroxyl groups, due to the formation of hydrogen bonds between hydroxyl groups in starch molecules, the granules are insoluble in water and also in gener...

Examples

Embodiment 1

[0039] Solid or gaseous SO 3 , add or pass into cooled 1,2-dichloroethane to form 4mol / L SO 3 / 1,2-dichloroethane solution. Then add starch into the reactor according to the amount in the table, at different SO 3 See Table 2, Table 3, Table 4, and Table 5 for the results of related experiments and comparative experiments on starch conversion rate under the conditions of dosage, 1,2-dichloroethane dosage, reaction time and reaction temperature.

[0040] Table 2: Different SOs 3 Yield of starch sulfate under dosage

[0041]

[0042]

[0043] Note: n U : n SO3 is the number of moles of starch unit structure and SO 3 The ratio of the number of moles, the precipitation temperature is below 30°C (the same below)

[0044] It can be seen that increasing the concentration and dosage of sulfur trioxide is conducive to improving the conversion rate of starch, but it is easy to cause degradation, resulting in increased loss of alcohol solubility during alcohol purification. ...

Embodiment 2

[0055] Solid or gaseous SO 3 , add or pass into cooled 1,2-dichloroethane to form 4mol / L SO 3 / 1,2-dichloroethane solution. Then take the pure product of soluble starch as raw material, and react according to the experimental conditions in Table 6, as the experimental contrast with wheat starch. The results of related experiments and control experiments are shown in Table 6.

[0056] Table 6 Exploration of the sulfation effect of different raw material starches

[0057]

[0058] This process system is suitable for raw materials from different sources and can obtain higher product yields.

Embodiment 3

[0060] Use 98% concentrated sulfuric acid to directly react with wheat flour or 98% concentrated sulfuric acid to react with wheat flour under the condition of ethanol dispersion. The results of related experiments and control experiments are shown in Table 7.

[0061] Table 7 H 2 SO 4 Sulfation effect of

[0062]

[0063] Under normal temperature conditions, the product yield and starch residual rate are very low, which shows that the carbonization of concentrated sulfuric acid is very serious.

technical field

[0001] The invention relates to a new synthesis process of starch sulfate and its salt, which belongs to the technical field of starch modification. Background technique

[0002] Starch is a high-molecular carbohydrate widely present in the roots, stems, seeds and other tissues of most plants. Amylose is mainly linked by D-glucopyranose via α-1,4 glycosidic bonds. It is a linear polymer; and amylopectin is a nonlinear polymer connected by α-1,4 glycosidic bonds and α-1,6 glycosidic bonds. There is an alcoholic hydroxyl group at the 2, 3, and 6 positions of each anhydroglucose unit in the starch molecule, and the primary hydroxyl group at the 6-position carbon atom has the highest activity, followed by the secondary hydroxyl groups at the 2nd and 3rd positions.

[0003] Although starch molecules are rich in hydroxyl groups, due to the formation of hydrogen bonds between hydroxyl groups in starch molecules, the granules are insoluble in water and also in gener...

Examples

Embodiment 1

[0039] Solid or gaseous SO 3 , add or pass into cooled 1,2-dichloroethane to form 4mol / L SO 3 / 1,2-dichloroethane solution. Then add starch into the reactor according to the amount in the table, at different SO 3 See Table 2, Table 3, Table 4, and Table 5 for the results of related experiments and comparative experiments on starch conversion rate under the conditions of dosage, 1,2-dichloroethane dosage, reaction time and reaction temperature.

[0040] Table 2: Different SOs 3 Yield of starch sulfate under dosage

[0041]

[0042]

[0043] Note: n U : n SO3 is the number of moles of starch unit structure and SO 3 The ratio of the number of moles, the precipitation temperature is below 30°C (the same below)

[0044] It can be seen that increasing the concentration and dosage of sulfur trioxide is conducive to improving the conversion rate of starch, but it is easy to cause degradation, resulting in increased loss of alcohol solubility during alcohol purification. ...

Embodiment 2

[0055] Solid or gaseous SO 3 , add or pass into cooled 1,2-dichloroethane to form 4mol / L SO 3 / 1,2-dichloroethane solution. Then take the pure product of soluble starch as raw material, and react according to the experimental conditions in Table 6, as the experimental contrast with wheat starch. The results of related experiments and control experiments are shown in Table 6.

[0056] Table 6 Exploration of the sulfation effect of different raw material starches

[0057]

[0058] This process system is suitable for raw materials from different sources and can obtain higher product yields.

Embodiment 3

[0060] Use 98% concentrated sulfuric acid to directly react with wheat flour or 98% concentrated sulfuric acid to react with wheat flour under the condition of ethanol dispersion. The results of related experiments and control experiments are shown in Table 7.

[0061] Table 7 H 2 SO 4 Sulfation effect of

[0062]

[0063] Under normal temperature conditions, the product yield and starch residual rate are very low, which shows that the carbonization of concentrated sulfuric acid is very serious.

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