CN110305229A - A kind of amphoteric starch and preparation method thereof - Google Patents
A kind of amphoteric starch and preparation method thereof Download PDFInfo
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- CN110305229A CN110305229A CN201810228918.XA CN201810228918A CN110305229A CN 110305229 A CN110305229 A CN 110305229A CN 201810228918 A CN201810228918 A CN 201810228918A CN 110305229 A CN110305229 A CN 110305229A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B31/00—Preparation of derivatives of starch
- C08B31/003—Crosslinking of starch
- C08B31/006—Crosslinking of derivatives of starch
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B31/00—Preparation of derivatives of starch
- C08B31/02—Esters
- C08B31/04—Esters of organic acids, e.g. alkenyl-succinated starch
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B31/00—Preparation of derivatives of starch
- C08B31/08—Ethers
- C08B31/12—Ethers having alkyl or cycloalkyl radicals substituted by heteroatoms, e.g. hydroxyalkyl or carboxyalkyl starch
- C08B31/125—Ethers having alkyl or cycloalkyl radicals substituted by heteroatoms, e.g. hydroxyalkyl or carboxyalkyl starch having a substituent containing at least one nitrogen atom, e.g. cationic starch
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B31/00—Preparation of derivatives of starch
- C08B31/16—Ether-esters
Abstract
The invention discloses a kind of preparation methods of macromolecule amphoteric starch, the following steps are included: opening mixer, starch is added, hydroxide sodium powder is then slowly added into be uniformly mixed, starch pH value 11.4-11.7 is adjusted, until 2 sub-samplings detect pH value difference < 0.2, chloro- 2 hydroxypropyl-trimethyl ammonium chloride of 3- after being activated with spraying mode addition with sodium hydroxide, 70 ± 2 DEG C are warming up to, insulation reaction 3h；PH value is adjusted to 11.0 ± 0.1,20-50 parts of monoxone powder are added, is uniformly mixed, reacts 3-4h at 75 ± 2 DEG C；0.3-1.0 part epoxychloropropane are added in 40 DEG C of cooling, spray pattern, react 1h, cool down 30 DEG C, in sulfuric acid or acetic acid and pH value is to 6.5-7.5, discharge.Amphoteric starch simple production process of the invention, reaction efficiency is high, and low energy consumption, and pollution is small, is suitble to the characteristics of preparing high substituted degree product.
Description
Technical field
The present invention relates to a kind of preparation methods of converted starch, and in particular to a kind of preparation side of macromolecule amphoteric starch
Method.
Background technique
2015, Chinese paper and paperboard production were about more than 11,000 ten thousand tons, and China becomes paper in the world and paperboard production is maximum
Country.Since network Development bring is impacted, newsprint sharply declines, and copper sheet, writing printing, white board slowly decline；Together
When, " internet+" also provides a new opportunity to develop to paper industry, and packaging industry is grown rapidly, boxboard and corrugation
Sustainable growth therewith.But China is the relatively deficient country of a forest resourceies, and China's afforestation rate only has global average water
Flat 2/3 comes the 139th, the world.0.145 hectare of area of woods per capita, the 1/4 of insufficient world occupancy volume per person；It is gloomy per capita
Woods accumulates 10.151 cubic metres, only the 1/7 of world occupancy volume per person, under severe Market Situation, package paper and paper kind
It is more and more to select waste paper pulp-making, very high requirement is proposed to paper making wet part.
With the increase of reuse number, swollen is substantially reduced after pulp beating, and fibre length reduces, and fines content increases
Add, secondary stock keratinization increases, and when waste paper recycling, the bond strength of fiber is substantially reduced, the water retention value decline of paper pulp, page
Thickness increases, and tightness, fracture length decline whiteness and opacity increased, light scattering coefficient decline.Therefore, for boxboard
The features such as smaller with fiber used in corrugated paper, macromolecule amphoteric starch is prepared, balance system charge passes through " bridge formation " of macromolecular
Effect, makes fiber fines are stable to be combined together, solves the problems, such as that boxboard and corrugated paper paper strength are poor, meanwhile, to mentioning
Rise the very helpful of paper machine operation performance.
Currently, the two kinds of ion denaturation of domestic amphoteric starch yin-yang, and molecular weight does not have much variations, production technology is mostly wet
Method production, is also easy to produce a large amount of waste water, pollutes the environment, and technique production procedure is long, high production cost.
Domestic amphoteric starch molecular weight does not have much variations relative to ative starch, is 10-30 ten thousand, degree ofacationic substitution does not surpass
0.040 is crossed, production technology is mostly wet production, and a large amount of waste water are also easy to produce, are polluted the environment, and dry production has technique
Simply, reaction efficiency is high, and low energy consumption, and pollution is small, is suitble to the characteristics of preparing high substituted degree product, therefore, studies its synthesis and property
Can, it is very significant to develop a kind of macromolecule amphoteric starch.
Summary of the invention
The object of the present invention is to provide a kind of amphoteric starches and preparation method thereof, can solve in the prior art above-mentioned
Disadvantage.
The invention adopts the following technical scheme:
A kind of preparation method of macromolecule amphoteric starch, comprising the following steps:
Mixer is opened, starch is added, hydroxide sodium powder is then slowly added into and is uniformly mixed, adjust starch pH value 11.4-11.7,
Until 2 sub-samplings detect pH value difference < 0.2, chloro- 2 hydroxypropyl three of 3- after being activated with spraying mode addition with sodium hydroxide
Ammonio methacrylate is warming up to 70 ± 2 DEG C, insulation reaction 3h；
PH value is adjusted to 11.0 ± 0.1,20-50 parts of monoxone powder are added, is uniformly mixed, reacts 3-4h at 75 ± 2 DEG C；
0.3-1.0 parts of epoxychloropropane are added in 40 DEG C of cooling, spray pattern, react 1h, cool down 30 DEG C, are neutralized with sulfuric acid or acetic acid
PH value discharges to 6.5-7.5.
Water-bath can not be sufficiently gelatinized under the starch normal pressure, it is necessary to carry out boiling gelatinization, continuous steaming with continuous steamer
Boiler use condition: boiling concentration 1-10%, back pressure 0.2-0.5 Mpa, 120-130 DEG C of temperature.
The amount of starch and the chloro- 2 hydroxypropyl-trimethyl ammonium chloride each component of 3- in the preparation method are as follows:
1000 parts of starch；
50-100 parts of 3- chloro- 2 hydroxypropyl-trimethyl ammonium chloride.
Raw starch is cornstarch, tapioca or potato starch or the mixture of three.
The molecular weight of the macromolecule amphoteric starch of this method production is 4-10 times of common amphoteric starch, cationic acquirement degree
For 0.02-0.05, Anion substituting degree 0.015-0.045.
A kind of amphoteric starch is prepared by above-mentioned preparation method.
The molecular weight of the amphoteric starch is 4-10 times of common amphoteric starch, and cationic acquirements degree is 0.02-0.05, it is negative from
Sub- degree of substitution is 0.015-0.045.
The invention has the advantages that amphoteric starch molecular weight of the invention does not have much variations relative to ative starch, it is 10-30
Ten thousand, degree ofacationic substitution is no more than 0.040, and production technology is mostly wet production, is also easy to produce a large amount of waste water, causes dirt to environment
Dye, and dry production has simple process, reaction efficiency is high, and low energy consumption, and pollution is small, is suitble to prepare the spy of high substituted degree product
Point.
Specific embodiment
The present invention may be implemented various change and have diversified form, will herein be described in detail realize example (or
Embodiment), but must not therefore limit the invention to specific announcement form, thought of the invention and technical scope included one
Shear, equipollent or even substitute should all be considered as the scope of the present invention.
Term used herein is only to illustrate specific implementation example (or embodiment) and use, and must not therefore limit to this hair
It is bright.Unless can significantly be distinguish in the pulse of sentence, otherwise singular manifestation mode also includes the situation of plural number.This Shen
The terms such as " comprising " please or " having " are only referred to the feature for determining to record on specification, number, step, movement, constituent element, zero
The presence of part or their combination is not construed as eliminating one or more other feature in advance, number, step, move
Work, constituent element, the presence of part or their combination or the presence of additional possibility.
Unless in addition give different definition, otherwise all arts as used herein including technology or scientific term
Meaning represented by language is identical with the meaning that the people in the technical field of the invention with general knowledge usually understand.One
As have in dictionary the meaning of defined term that should be interpreted and the meaning according to possessed by the article pulse of the relevant technologies
Unanimously, it defines unless clearly giving in this application, otherwise singularly or excessively must not make an explanation to formalism.
" first " recorded in this specification, " second " etc. only indicate mutually different constituent element, not by manufacturing sequence
Limitation, detailed description of the invention and its title in claims may be inconsistent.
Starch is a kind of important renewable and biodegradable natural resources, has many hydroxyls on starch molecule,
Under the conditions of certain temperature, can water swelling and be gelatinized, have certain viscosity and adhesion strength, industrially have wide answer
With.
It is higher to the Functional Requirement of starch product with the development of paper industry, if required better film forming, glue
Spend the performances such as stability high, permeability is strong, cohesive force is good, anti-aging, resistant to shearing.Amphoteric starch is the principal item of converted starch
One of, refer to and be not only connected to cation group in starch chain, but also connect the converted starch of anionic group, have cationic starch,
The multiplets such as anionic starch, natural polymers and characteristic, service performance is more than single converted starch derivative
It is superior.
Compared with common unitary converted starch, composite modified starch is as paper making wet part additive, and effect is than independent
Good using unitary converted starch, amphoteric starch is exactly one of composite modified starch Typical Representative.Cationic starch is starch ether
A kind of important derivatives can combine closely since it has positive charge with negatively charged fiber fines, filler, thus extensively
Paper quality can be significantly improved, consumption is reduced, reduces cost as enhancing, retention, filter aid applied to paper making wet part.Sun from
It is the sub- starch huge market demand, various in style, can be divided by the structure of its amino-compound: tertiary amine-type, quaternary ammonium type, primary amine type,
The cationic starches such as secondary amine type and miscellany (such as imines), wherein quaternary ammonium cation starch is in the extensive pH such as neutrality, alkalinity
It can be used and be stabilized under range, therefore there is biggish commodity value.Cationic starch with high substitution degree is in wet end of machine
Interference of the removal anionic species to papermaking can be neutralized.The reagent for leading to common starch positive ionization is that quaternary ammonium type 3- is chloro-
2- hydroxypropyl-trimethyl ammonium chloride etherifying reagent.This etherifying reagent is under acid, neutral, alkaline condition, all aobvious cation state.Depending on
The difference of its anionic group can be divided into the composite starch such as phosphatic type, carboxyl type, sulfonic acid type and sulfuric acid type and xanthan acid type, compound
The cation group of converted starch is generally tertiary amine or quaternary ammonium salt.
The mechanism of action of the multicomponent modified starch such as amphoteric starch in papermaking:
(1) paper-making fibre is usually negatively charged, thus is easy to Liquidity limit auxiliary agent, but be also easy to adsorb other positively charged objects
Matter thus weakens absorption of the fiber to cationic auxiliary, and the anionic group of multicomponent modified starch itself can preferentially be inhaled
Positively charged substance in attached system, the absorption to avoid these electropositive substances to paper-making fibre.
(2) the anionic group of multicomponent modified starch itself can shield to cation group, electric exclusion those
The high activity present in system " miscellaneous anion ", thus make the cation group in auxiliary agent will not occur it is premature reaction or by
It neutralizes；Equally, cation also protects anion, the coordinative role of this positive and negative ionic group, so as to " miscellaneous " yin, yang is contained
Straw pulp, secondary stock and Newsprint Pulp more than ion interference have apparent application effect (to form sediment relative to anionic starch and cation
For powder).
(3) non-ionic substituent often plays the role of synergy.Adhesion, enhancing of the non-ionic group in addition to playing itself
The effects of outside, can also play the role of shielding electrostatic attraction to anions and canons group, and coordinate.Thus, compare on application performance
Macromolecule amphoteric starch effect is more stable.
(4) in neutral or alkaline copy paper, the balance susceptibility of ionic charge is larger, and system is easier to cation occurred
Change, cause wet end out of control, and the charge balance of system can be made to be controlled using multicomponent modified starch.
(5) the stability of multicomponent modified starch storage is good, non-aging.This is because in molecule containing yin, yang and it is non-from
Subbase group, it is not easy to form straight chain haptophore, even therefore 0.25% weak solution, will not aging.
(6) the charge of multicomponent modified starch is in a basic balance, when the starch that do not kept is recycled after being discharged with water, no
Charge balance can be lost, to can guarantee the good operating condition of paper machine.The number of additional amount will not influence in the paper making process
The Zeta current potential of paper pulp, paper plant can be added as needed until satisfied.
Example 1
A. mixer is opened, 1000 parts of starch are added, hydroxide sodium powder is then slowly added into and is uniformly mixed, adjust starch pH value
11.6, until 2 sub-samplings detect pH value difference < 0.2, chloro- 2 hydroxyl of 3- after being activated with spraying mode addition with sodium hydroxide
70 parts of hydroxypropyltrimonium chloride, 70 DEG C are warming up to, insulation reaction 3h.
B. 30 parts of monoxone powder are added to 11.0 in adjustment pH value, are uniformly mixed, react 3-4h at 75 DEG C.
C. cool down 40 DEG C, 0.6 part of epoxychloropropane is added in spray pattern, reacts 1h, cools down 30 DEG C, with sulfuric acid or acetic acid
PH value is neutralized to 7.0, is discharged.
The molecular weight of the macromolecule amphoteric starch of this method production is 7 times of common amphoteric starch, and cationic acquirement degree is
0.035, Anion substituting degree 0.025 has obvious action, waste water to enhancings such as boxboard, corrugated paper, paper jam, paperboards
The content of middle COD reduces by 15%.
Example 2
A. mixer is opened, 1000 parts of starch are added, hydroxide sodium powder is then slowly added into and is uniformly mixed, adjust starch pH value
11.7, until 2 sub-samplings detect pH value difference < 0.2, chloro- 2 hydroxyl of 3- after being activated with spraying mode addition with sodium hydroxide
60 parts of hydroxypropyltrimonium chloride, 70 DEG C are warming up to, insulation reaction 3h.
B. 30 parts of monoxone powder are added to 11.1 in adjustment pH value, are uniformly mixed, react 3-4h at 75 DEG C.
C. cool down 40 DEG C, 0.7 part of epoxychloropropane is added in spray pattern, reacts 1h, cools down 30 DEG C, with sulfuric acid or acetic acid
PH value is neutralized to 6.8, is discharged.
The molecular weight of the macromolecule amphoteric starch of this method production is 9 times of common amphoteric starch, and cationic acquirement degree is
0.028, Anion substituting degree 0.025 has obvious action, waste water to enhancings such as boxboard, corrugated paper, paper jam, paperboards
The content of middle COD reduces by 18%.
Example 3
A. mixer is opened, 1000 parts of starch are added, hydroxide sodium powder is then slowly added into and is uniformly mixed, adjust starch pH value
11.5, until 2 sub-samplings detect pH value difference < 0.2, chloro- 2 hydroxyl of 3- after being activated with spraying mode addition with sodium hydroxide
100 parts of hydroxypropyltrimonium chloride, 70 DEG C are warming up to, insulation reaction 3h.
B. 50 parts of monoxone powder are added to 11.0 in adjustment pH value, are uniformly mixed, react 3-4h at 75 DEG C.
C. cool down 40 DEG C, 1 part of epoxychloropropane is added in spray pattern, reacts 1h, cools down 30 DEG C, in sulfuric acid or acetic acid
With pH value to 7.0, discharging.
The molecular weight of the macromolecule amphoteric starch of this method production is 10 times of common amphoteric starch, and cationic acquirement degree is
0.059, Anion substituting degree 0.044 has obvious action, waste water to enhancings such as boxboard, corrugated paper, paper jam, paperboards
The content of middle COD reduces by 21%.
Example 4
A. mixer is opened, 1000 parts of starch are added, hydroxide sodium powder is then slowly added into and is uniformly mixed, adjust starch pH value
11.5, until 2 sub-samplings detect pH value difference < 0.2, chloro- 2 hydroxyl of 3- after being activated with spraying mode addition with sodium hydroxide
50 parts of hydroxypropyltrimonium chloride, 70 DEG C are warming up to, insulation reaction 3h.
B. 30 parts of monoxone powder are added to 11.0 in adjustment pH value, are uniformly mixed, react 3-4h at 75 DEG C.
C. cool down 40 DEG C, 0.3 part of epoxychloropropane is added in spray pattern, reacts 1h, cools down 30 DEG C, with sulfuric acid or acetic acid
PH value is neutralized to 6.8, is discharged.
The molecular weight of the macromolecule amphoteric starch of this method production is 4 times of common amphoteric starch, and cationic acquirement degree is
0.021, Anion substituting degree 0.016 has obvious action, waste water to enhancings such as boxboard, corrugated paper, paper jam, paperboards
The content of middle COD reduces by 12%.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within mind and principle.
Claims (7)
1. a kind of preparation method of the macromolecule amphoteric starch of claim 1, which comprises the following steps:
Mixer is opened, starch is added, hydroxide sodium powder is then slowly added into and is uniformly mixed, adjust starch pH value 11.4-11.7,
Until 2 sub-samplings detect pH value difference < 0.2, chloro- 2 hydroxypropyl three of 3- after being activated with spraying mode addition with sodium hydroxide
Ammonio methacrylate is warming up to 70 ± 2 DEG C, insulation reaction 3h；
PH value is adjusted to 11.0 ± 0.1,20-50 parts of monoxone powder are added, is uniformly mixed, reacts 3-4h at 75 ± 2 DEG C；
0.3-1.0 parts of epoxychloropropane are added in 40 DEG C of cooling, spray pattern, react 1h, cool down 30 DEG C, are neutralized with sulfuric acid or acetic acid
PH value discharges to 6.5-7.5.
2. the preparation method of the macromolecule amphoteric starch according to claim 1 of claim 2, which is characterized in that the shallow lake
Water-bath can not be sufficiently gelatinized under powder normal pressure, it is necessary to carry out boiling gelatinization with continuous steamer, continuous steamer use condition:
Boiling concentration 1-10%, back pressure 0.2-0.5 Mpa, 120-130 DEG C of temperature.
3. the preparation method of the macromolecule amphoteric starch according to claim 2 of claim 3, which is characterized in that
The amount of starch and the chloro- 2 hydroxypropyl-trimethyl ammonium chloride each component of 3- in the preparation method are as follows:
1000 parts of starch；
50-100 parts of 3- chloro- 2 hydroxypropyl-trimethyl ammonium chloride.
4. the preparation method of the macromolecule amphoteric starch according to claim 3 of claim 4, which is characterized in that
Raw starch is cornstarch, tapioca or potato starch or the mixture of three.
5. the preparation method of the macromolecule amphoteric starch according to claim 4 of claim 5, which is characterized in that the party
The molecular weight of the macromolecule amphoteric starch of method production is 4-10 times of common amphoteric starch, and cationic acquirement degree is 0.02-0.05,
Anion substituting degree is 0.015-0.045.
6. a kind of amphoteric starch of claim 6, which is characterized in that its preparation side for passing through any one of Claims 1-4
Method is prepared.
7. the amphoteric starch according to claim 5 of claim 7, which is characterized in that the molecular weight of the amphoteric starch is
4-10 times of common amphoteric starch, cationic acquirement degree are 0.02-0.05, Anion substituting degree 0.015-0.045.
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| CN103509128A (en) * | 2013-09-05 | 2014-01-15 | 江西顺昌隆实业有限公司 | One-step preparation method for carboxyl-type amphoteric starch by employing semi-dry technology |
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2018
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| CN1939932A (en) * | 2006-06-23 | 2007-04-04 | 中国科学院成都有机化学有限公司 | Synthesis of soluble amphoteric starch |
| CN103242459A (en) * | 2013-05-27 | 2013-08-14 | 江西鑫川实业有限公司 | Crosslinked amphoteric starch and preparation method thereof |
| CN103435708A (en) * | 2013-09-05 | 2013-12-11 | 长沙理工大学 | Preparation method of nanometer amphoteric starch |
| CN103509128A (en) * | 2013-09-05 | 2014-01-15 | 江西顺昌隆实业有限公司 | One-step preparation method for carboxyl-type amphoteric starch by employing semi-dry technology |
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