CN100408598C - Composite modified starch and its preparing method - Google Patents
Composite modified starch and its preparing method Download PDFInfo
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- CN100408598C CN100408598C CNB2004100366279A CN200410036627A CN100408598C CN 100408598 C CN100408598 C CN 100408598C CN B2004100366279 A CNB2004100366279 A CN B2004100366279A CN 200410036627 A CN200410036627 A CN 200410036627A CN 100408598 C CN100408598 C CN 100408598C
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Abstract
The present invention relates to a composite modified starch and a preparing method thereof. Firstly, the starch is regulated into slurry by alcohol and water mixed liquid, and alkaline liquid and a crosslinking agent are added so that the starch reacts with the crosslinking agent. Secondly, sodium chloroacetate and the alkaline liquid are added to carry out carboxymethylation reaction, or the sodium chloroacetate and the crosslinking agent are directly added into the starch slurry, and the alkaline liquid is added to carry out carboxymethylation and crosslinking reaction. After the reaction ends, the materials are conveyed into a pre-gelatinization drying machine to further react, and the materials are dried, pulverized and packed to obtain the new modified starch. In the present invention, the beneficial conditions of methods of pre-gelatinization, carboxymethylation, crosslinking etherification and the like are integrated. The prepared composite modified starch has the characteristics of stable viscosity, cold water solubility, good water absorption, strong rehydration, shearing force resistance, strong alkali resistance, high freezing stability, freezing and thawing stability, no coagulation and sedimentation, good film forming performance, etc. A product with high viscosity can be manufactured by adjusting the number of the crosslinking agent by the method. The product with high viscosity is used as adhesive in construction plastering and the preparation of paint, petroleum well drilling, toothpaste and ceramics. A prepared product with low viscosity is used as a water keeping agent of agriculture and forestry, and an absorbent of sanitary facial tissues, napkins, etc.
Description
Technical field
The present invention relates to chemical glue stick technical field, specifically a kind of composite modified starch.
Background technology
In the prior art, one or both denaturation methods among pre-gelatinization, carboxymethyl etherification, the crosslinked etherificate three are adopted in the sex change of starch mostly.Wherein:
Pre-gelatinized starch can swelling dissolve in cold water, and rehydration is good, but its cold bonding degree is lower, easily retrogradation.
Carboxymethyl starch dissolves in cold water at substitution value more than 0.1, the solution clear, and viscosity is also high, and bonding force is big, and solvability is good; But its viscosity anti-shearing force is poor, has influenced its use range greatly, and is very responsive to salt, adds small amount of hydrochloric acid in solution, sodium hydroxide solution will make viscosity drop much lower.
The cross-linking starch anti-shearing force is strong, and can change the viscose glue of starch paste, has higher freeze-stable and freeze-thaw stability, but its cold water solubility is poor.
So far do not retrieve the preparation method who above-mentioned three kinds of methods is merged, makes starch generation complex reaction and generate modified starch as yet.
Summary of the invention
The object of the present invention is to provide a kind of pre-gelatinization, carboxymethyl etherification and three kinds of reaction methods of crosslinked etherificate to be blended in the method for preparing composite modified starch of one, it makes starch generation complex reaction, generates a kind of new composite modified starch.This composite modified starch stable viscosity; Cold water solubles; Good water absorption, rehydration are strong; Anti-shearing force, anti-highly basic; Have higher freeze-stable and freeze-thaw stability; Not retrogradation; Good film-forming property.
The foregoing invention purpose is achieved through the following technical measures:
A kind of composite modified starch, its raw material comprises starch, linking agent, sodium hydroxide, sodium chloroacetate, alcohol and water, its basal component in the parts by weight proportioning is:
100 parts of starch
0.005～5 part of linking agent
1～20 part in sodium hydroxide
5～50 parts of sodium chloroacetates
50～1000 parts of alcohol
50～1000 parts in water
First kind of preparation method: according to above-mentioned each set of dispense ratio, with starch is that 10%～98% alcohol-water mixture furnishing powder is starched with weight percent earlier, add weight percent again and be 1%～45% described alkali lye and linking agent, under 1～45 ℃, make starch and linking agent reaction 0.3～4 hour, add described sodium chloroacetate then, and be that to regulate pH be 10～13 for 1%～45% alkali lye with weight percent, under 1～100 ℃, carried out carboxymethylation reaction 1～100 hour, after reaction finishes, import pre-gelatinization drying machine 150～180 ℃ of further reactions down, crushed after being dried, packing promptly at last.
Second kind of preparation method: according to above-mentioned each set of dispense ratio, with starch is that 10%～98% alcohol-water mixture furnishing powder is starched with weight percent earlier, directly in starch slurry, add sodium chloroacetate and linking agent, add weight percent again and be 1%～45% described alkali lye, and be that to regulate pH be 10～13 for 1%～45% alkali lye with weight percent, carried out carboxymethyl and crosslinking reaction 1～100 hour, after reaction finishes, import pre-gelatinization drying machine 150～180 ℃ of further reactions down, crushed after being dried, packing promptly at last.
For make the composite modified starch post-production and use convenient, on the basis of above-mentioned basic recipe, treat that carboxymethyl and crosslinking reaction finish after, add 0.1～10 part in urea, 0.1～5 part of glycerine, import pre-gelatinization drying machine again and further react, crushed after being dried, packing is promptly at last.
Linking agent comprises formaldehyde, propenal, succinic aldehyde, melamino-for maldehyde or epoxy chloropropane, phosphoryl chloride, carbonic acid chlorine, Ethylene Dichloride, β, β '-dichloro-diethyl ether, aliphatics dihalide compound, cyanuryl chloride or urea, dimethylolurea, dihydroxymethyl ethylene urea, N, N-methylene diacrylamine or urea formaldehyde resins in the described prescription.
Among the preparation method of above-mentioned modified starch, reacting used alcohol is methyl alcohol, ethanol, propyl alcohol or Virahol.Starch is wheat, corn, cassava or yam starch.
Composite modified starch provided by the invention, the advantage of having integrated pre-gelatinization, carboxymethyl etherification and three kinds of methods of crosslinked etherificate in its preparation method is in one, and the composite modified starch of preparation has stable viscosity; Cold water instant dissolving; Good water absorption, rehydration are strong; Anti-shearing force, anti-highly basic; Have higher freeze-stable and freeze-thaw stability; Not retrogradation; Characteristics such as good film-forming property.In addition, this method is by adjusting the quantity of linking agent, can produce full-bodied product, raw material as tackiness agent uses, its viscosity height, and bonding force is strong, mutually solvent with other water-soluble glue, and its collodion silk is " short silk ", these characteristics building whitewash and coating, petroleum drilling, toothpaste, ceramic making in use as tackiness agent, incomparable advantage is arranged.Also can produce low viscous product, utilize its good water absorption, the characteristics that rehydration is strong are as the agroforestry water-holding agent; Sanitary paper towel, diaper etc. are as absorption agent.
Embodiment
Embodiment 1: in the stirred vessel, add 1000 parts water and 700 part 95% ethanol, add 1000 parts of starch again, stir into the powder slurry, add 100 part of 5% liquid caustic soda, 0.05 part of cyanuryl chloride makes starch and linking agent react under 20～25 ℃ about 2 hours; Add 350 parts of 98% sodium chloroacetates again, it is 10～11 that the alkali lye with 35% is adjusted pH value, carries out carboxymethylation reaction 4 hours under 50 ℃; After reaction finishes, add 5 parts in urea, 5 parts of glycerine are transported to pre-gelatinization drying machine, and adjusting temperature on pre-gelatinization drying machine is 150～180 ℃, and the gelatinization reaction is after 1～10 minute once more; Drying, pulverizing, packing.Product is irregular flakey, 2% solution viscosity η=1000～2500mpa.s, and substitution value D.S.＞0.1, cold water is easily molten, and solution is transparent, and 20 days are not stratified.
Embodiment 2: water and 800 part of 90% propyl alcohol of adding 1000 parts in stirred vessel, add 1000 parts of starch again, stir into the powder slurry, add 80 part of 10% liquid caustic soda, 0.05 part of cyanuryl chloride, 20～25 ℃ were reacted 2 hours, added 330 parts of 98% sodium chloroacetates again, and it is 10～11 that the alkali lye with 35% is adjusted pH value, under 50 ℃, carried out carboxymethylation reaction 4 hours, after reaction finishes, add 8 parts in urea, 4 parts of glycerine, being transported to and adjusting temperature on the pre-gelatinization drying machine is 150～180 ℃, the gelatinization reaction is after 1～10 minute once more, and drying and crushing is packed, and product design and performance are close with embodiment 1.
Embodiment 3: in stirred vessel, water and 700 part of 95% Virahol of adding 1000 parts, add 1000 parts of starch again, stir into the powder slurry, add 50 part of 10% liquid caustic soda, 0.05 part of cyanuryl chloride, 20～25 ℃ of reactions 2 hours, add 350 part of 98% sodium chloroacetate again, add 8 parts in urea, 4 parts of glycerine, alkali lye with 35% is adjusted pH value 10～13, carried out carboxymethylation reaction 4 hours under 50 ℃, reaction is transported to pre-gelatinization drying machine after finishing, adjusting temperature on pre-gelatinization drying machine is 150～180 ℃, the gelatinization reaction is after 1～10 minute once more, and drying and crushing is packed, and product design and performance are close with embodiment 1.
Among the embodiment 1-3, aldehydes such as the formaldehyde of linking agent cyanuryl chloride usefulness equivalent, propenal, succinic aldehyde, melamino-for maldehyde; Or epoxy chloropropane, phosphoryl chloride, carbonic acid chlorine, Ethylene Dichloride, β, halogenide such as β '-dichloro-diethyl ether, aliphatics dihalide compound; Or amino imino compounds such as urea, dimethylolurea, dihydroxymethyl ethylene urea, N, N-methylene diacrylamine, urea formaldehyde resins replace, and products obtained therefrom profile and performance are close with embodiment 1.
Embodiment 4: in stirred vessel, water and 700 part of 95% ethanol of adding 1000 parts, add 1000 parts of starch again, stir into the powder slurry, add 50 part of 10% liquid caustic soda, 25 parts in formaldehyde was 38～40 ℃ of reactions 4 hours, add 350 part of 98% sodium chloroacetate again, alkali lye with 35% is adjusted pH value 10～13, carries out carboxymethylation reaction 4 hours under 50 ℃, after reaction finishes, add 8 parts in urea, 4 parts of glycerine are transported to pre-gelatinization drying machine, and adjusting temperature on pre-gelatinization drying machine is 150～180 ℃, the gelatinization reaction is after 1～10 minute once more, and drying and crushing is packed.Product is irregular flakey, 2% solution viscosity η=100～1000mpa.s, and substitution value D.S.＞0.1, cold water is easily molten, and 20 days are not stratified.
Among the embodiment 4, aldehydes such as the propenal of linking agent formaldehyde usefulness equivalent, succinic aldehyde, melamino-for maldehyde; Or epoxy chloropropane, phosphoryl chloride, carbonic acid chlorine, Ethylene Dichloride, β, halogenide such as β '-dichloro-diethyl ether, aliphatics dihalide compound, cyanuryl chloride; Or amino imino compounds such as urea, dimethylolurea, dihydroxymethyl ethylene urea, N, N-methylene diacrylamine, urea formaldehyde resins replace, and products obtained therefrom profile and performance are close with embodiment 4.
Embodiment 5: in stirred vessel, add water and 700 part of 95% ethanol of 1000 parts, add 1000 parts of starch again, stir into the powder slurry, add 50 part of 10% liquid caustic soda, 5 parts of epoxy chloropropane were 20～25 ℃ of reactions 2 hours, add 350 part of 98% sodium chloroacetate again, alkali lye with 35% is adjusted pH value 10～13, carries out carboxymethylation reaction 4 hours under 50 ℃, after reaction finishes, add 8 parts in urea, 4 parts of glycerine are transported to pre-gelatinization drying machine, and adjusting temperature on pre-gelatinization drying machine is 150～180 ℃, the gelatinization reaction is after 1～10 minute once more, the drying and crushing packing, product design is irregular flakey, 2% solution viscosity η≤100mpa.s, substitution value D.S.＞0.1, cold water swelling, absorption speed are no more than 10 minutes, 20～23 times of water-intake rates, release outlet capacity and reach 98%, at average 9.62g/cm
2Pressure down can keep 87% moisture.
Among the embodiment 5, aldehydes such as the formaldehyde of linking agent epoxy chloropropane usefulness equivalent, propenal, succinic aldehyde, melamino-for maldehyde; Or phosphoryl chloride, carbonic acid chlorine, Ethylene Dichloride, β, halogenide such as β '-dichloro-diethyl ether, aliphatics dihalide compound, cyanuryl chloride; Or amino imino compounds such as urea, dimethylolurea, dihydroxymethyl ethylene urea, N, N-methylene diacrylamine, urea formaldehyde resins replace, and products obtained therefrom profile and performance are close with embodiment 5.
Embodiment 6: in stirred vessel, water and 700 part of 95% ethanol of adding 1000 parts, add 1000 parts of starch again, stir into the powder slurry, add 50 part of 10% liquid caustic soda, 50 parts of dimethylolurea, 20～25 ℃ of reactions 2 hours, add 350 part of 98% sodium chloroacetate again, add 4 parts in urea, 4 parts of glycerine, alkali lye with 35% is adjusted pH value 10～13, carried out carboxymethylation reaction 4 hours under 50 ℃, reaction is transported to pre-gelatinization drying machine after finishing, adjusting temperature on pre-gelatinization drying machine is 130～140 ℃, the gelatinization reaction is after 1～10 minute once more, and drying and crushing is packed, and product design and performance are close with embodiment 5.
Among the embodiment 6, aldehydes such as the formaldehyde of linking agent dimethylolurea usefulness equivalent, propenal, succinic aldehyde, melamino-for maldehyde; Or epoxy chloropropane, phosphoryl chloride, carbonic acid chlorine, Ethylene Dichloride, β, halogenide such as β '-dichloro-diethyl ether, aliphatics dihalide compound, cyanuryl chloride; Or amino imino compounds such as urea, dihydroxymethyl ethylene urea, N, N-methylene diacrylamine, urea formaldehyde resins replace, and products obtained therefrom profile and performance are close with embodiment 5.
Among above-mentioned all embodiment, starch can be selected wheat, corn, cassava, yam starch etc.
Claims (6)
1. a composite modified starch is characterized in that the basal component for preparing this composite modified starch comprises starch, linking agent, sodium hydroxide, sodium chloroacetate, alcohol and water, and its basal component in the parts by weight proportioning is:
100 parts of starch
0.005～5 part of linking agent
1～20 part in sodium hydroxide
5～50 parts of sodium chloroacetates
50～1000 parts of alcohol
50～1000 parts in water
According to above-mentioned each set of dispense ratio, with starch is that 10%～98% alcohol-water mixture furnishing powder is starched with weight percent earlier, add weight percent again and be 1%～45% alkali lye and linking agent, under 1～45 ℃, make starch and linking agent reaction 0.3～4 hour, add described sodium chloroacetate then, and be that to regulate pH be 10～13 for 1%～45% alkali lye with weight percent, under 1～100 ℃, carried out carboxymethylation reaction 1～100 hour, after reaction finishes, import pre-gelatinization drying machine 150～180 ℃ of further reactions down, crushed after being dried, packing promptly at last.
2. a composite modified starch is characterized in that the basal component for preparing this composite modified starch comprises starch, linking agent, sodium hydroxide, sodium chloroacetate, alcohol and water, and its basal component in the parts by weight proportioning is:
100 parts of starch
0.005～5 part of linking agent
1～20 part in sodium hydroxide
5～50 parts of sodium chloroacetates
50～1000 parts of alcohol
50～1000 parts in water
According to above-mentioned each set of dispense ratio, with starch is that 10%～98% alcohol-water mixture furnishing powder is starched with weight percent earlier, directly in starch slurry, add described sodium chloroacetate and linking agent, add weight percent again and be 1%～45% alkali lye, and be that to regulate pH be 10～13 for 1%～45% alkali lye with weight percent, carried out carboxymethylation and crosslinking reaction 1～100 hour, after reaction finishes, import pre-gelatinization drying machine 150～180 ℃ of further reactions down, crushed after being dried, packing promptly at last.
3. modified starch according to claim 1 and 2, it is characterized in that above-mentioned carboxymethylation and crosslinking reaction finish after, add 0.1～10 part in urea, 0.1～5 part of glycerine, import pre-gelatinization drying machine again and further react, crushed after being dried, packing promptly at last.
4. modified starch according to claim 1 and 2 is characterized in that linking agent comprises formaldehyde, propenal, succinic aldehyde, melamino-for maldehyde or epoxy chloropropane, phosphoryl chloride, carbonic acid chlorine, Ethylene Dichloride, β, β '-dichloro-diethyl ether, aliphatics dihalide compound, cyanuryl chloride or urea, dimethylolurea, dihydroxymethyl ethylene urea, N, N-methylene diacrylamine or urea formaldehyde resins in the described prescription.
5. modified starch according to claim 1 and 2 is characterized in that alcohol is methyl alcohol, ethanol, propyl alcohol or Virahol in the described prescription.
6. modified starch according to claim 1 and 2 is characterized in that starch is wheat, corn, cassava or yam starch in the described prescription.
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