CN1318694C - Hydroxyalkyl cationic guar gum and its preparation method and application - Google Patents
Hydroxyalkyl cationic guar gum and its preparation method and application Download PDFInfo
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Abstract
The present invention discloses a method of preparing hydroxyalkyl cationic guar gum and the application of the hydroxyalkyl cationic guar gum for pulp retention filter aid. The present invention has the preparing method that the initial powder of guar gum which is not purified is dispersed in low-carbon alcohol / aqueous solution and is soaked under the condition of alkalinity catalyst first, a cationic etherifying agent is added then to carry out the guar gum cationic graftingf reaction, phase-transfer catalyst and an alkoxy etherifying agent are added then to carry out the guar gum hydroxyalkyl reaction, and finally, hydroxyalkyl cationic guar gum is prepared by the steps of neutralization, filtering, etc. The preparing method has the advantages of simple production technique, less device investment, mild reaction condition and low production cost, and the cationic substitution degree of prepared products is high. When the hydroxyalkyl cationic guar gum is used as the pulp retention filter aid, the hydroxyalkyl cationic guar gum is formulated into water solution first and is filled in pulp suspension then; the application method has the advantages of little filling quantity, convenient operation, biodegradation resistance, stable viscosity, etc.
Description
Technical field
The present invention relates to paper pulp and use the retention and drainage aid agent field, specifically is manufacture paper with pulp retention and drainage aid agent in the process of feedstock production secondary stock, wood pulp and straw pulp system and high-grade functional paper with the guar gum, particularly relates to one-step slurry preparation method of hydroxylalkyl cationic guar gum.
Background technology
Paper industry widespread usage modified starch and cationic polyacrylamide (CPAM) are as retention and drainage aid agent at present, but differ in domestic starch material source, of a great variety, straight chain and amylopectin ratios are different, therefore have a strong impact on its modified product quality of stability, limited it and applied.The wet end adjuvant of external major company production is haveed no alternative but select for use in domestic big paper mill, causes paper cost to increase.On the other hand, cationic polyacrylamide is easily biological-degradable not, and residual monomer has certain toxicity, is restricted in the application of paper for daily use and high-grade paper.And the plain boiled water reuse meeting that contains CPAM causes the positive electricity enrichment, and the fleeces group of congealing into influences formation of sheet and the stability of the system that manufactures paper with pulp.
Guar gum is a kind of natural galactomannan gum, extracts to obtain from the endosperm of the guar seed that originates in ground such as India, Pakistan.The guar gum main chain is that the unit connection forms by (1,4) β-D mannose, and side chain is made up of single α-D galactolipin and is joined with (1,6) key and main chain.Its molecular structure similar with cellulose has determined it and the natural sympathy of cellulose.Guar gum is used for paper industry, and when improving paper fiber fines and filler retention and drainage effect, thereby the evenness that does not influence paper does not reduce its strength character.In recent years, since the plantation of guar gum, harvesting, purifying is pulverized and is realized industrialization, and the price advantage of its raw material makes first appearance.And the outstanding biodegradability of guar gum has been alleviated the problem of environmental pollution of paper industry, meets the cleaner production theory.
Be based on its application purpose about recent Progress in Modification of Guar Gum and carry out, the guar gum of modification is mainly at household chemicals, oil field chemical, and aspects such as mining, and obtain the approval of large-scale market.Disclose a kind of modified guar that contains anion, cationic substituent as U.S. Pat P5733854, the aqueous solution of the patented product has excellent light transmission and is applied to the abluent prescription.U.S. Pat P3326890, USP3350186, USP3483121 disclose the preparation technology of hydroxyalkyl guar gum.But the subject matter that these patented technologies exist is the synthesis step complexity, and the product substitution value is on the low side, does not also have to disclose the method that it uses as the paper pulp retention and drainage aid agent.
Summary of the invention
Purpose of the present invention is exactly in order to solve above-mentioned the deficiencies in the prior art part, provides a step puddling to prepare the preparation method of hydroxyalkyl cationic guar gum.
The object of the invention is achieved through the following technical solutions:
One step slurrying method of hydroxyalkyl cationic guar gum comprises the steps and process conditions:
(1) guar gum soaks alkalization, in mass fraction, 100 parts of former powder of not purified guar gum are joined in 200～880 parts of alcohol/aqueous mixtures, filling under the nitrogen condition, adding 20～100 parts of the aqueous solution of concentration 10%～100% base catalyst subsequently, soaking alkalization 0.5～1.5h, make alkalization guar gum suspension, the alcohol of described alcohol/aqueous mixtures is 1～10: 1 with the quality ratio, and described alcohol is methyl alcohol, absolute ethyl alcohol, industrial alcohol, isopropyl alcohol or the tert-butyl alcohol;
(2) guar gum cation graft reaction, in mass fraction, be that 50～70% cationic etherifying agent aqueous solution join in the alkalization guar gum suspension of step (1) gained with 10～100 parts of concentration, be under 35～75 degree conditions in temperature, reacted 2～6 hours, and made cationic intermediates;
(3) guar gum hydroxyalkylation reaction, in mass fraction, 0～10 portion of phase transfer catalyst is joined in the cationic intermediates of step (2) gained, fill nitrogen, vacuumize and-0.1～0.1MPa pressure condition under, add 20～100 portions of alkoxyl etherifying agents, replenish 0～25 part of 60% sodium hydroxide solution, exothermic heat of reaction makes spontaneous 40～75 degree that are raised to of temperature of charge, reacted 1～5 hour, cool to room temperature subsequently, and regulate material pH value to 7.0～8.5 with acidic materials, make with the mud state and be dispersed in hydroxyalkylation cation guar gum in alcohol/aqueous solution;
(4) step (3) the muddy attitude that is able to is dispersed in alcohol/aqueous solution the hydroxyalkylation cation guar gum after filtration, washing, dry, pulverize after, make hydroxyalkyl cationic guar gum.
The used base catalyst of step in the technique scheme (1), the used cationic etherifying agent of step (2), phase transfer catalyst that step (3) is used and alkoxyl etherifying agent are base catalyst general in such technology, cationic etherifying agent, phase transfer catalyst and alkoxyl etherifying agent, the preferred base catalyst of the present invention is a NaOH, potassium hydroxide, sodium methoxide, a kind of in the caustic alcohol and more than one mixture, the preferred cation etherifying agent is a 3-chloro-2-Hydroxyproyl Trimethyl ammonium chloride, the arsenic thiamine hydrochloride, quinoline hydrochloride or epoxypropyl trimethylammonium chloride amine, preferred phase transfer catalyst is a hexadecyl benzyl dimethly ammonium chloride, and preferred alkoxyl etherifying agent is an oxirane, expoxy propane, epoxy butane or chlorethanol or 2-chloropropyl alcohol.
Realize purpose of the present invention for better, the alcohol of alcohol/aqueous mixtures and quality are than preferred 1.2～9 in the described step (1): 1; Preferred 45～70 degree of described step (2) reaction temperature, preferred 2.5～5 hours of reaction time; In preferred 1.5～4.0 hours of the reaction time in the described step (3), regulate the used preferred hydrochloric acid of acidic materials of material pH value, acetic acid, boric acid, citric acid.
Hydroxyalkyl cationic guar gum preparation method of the present invention has the feature of a step puddling, be that melon glue alkalizes in alcohol/aqueous alkali, drop into cationic etherifying agent then and carry out the cation graft reaction, the intermediate that is obtained needn't purifies and separates, directly with the reaction of alkoxyl etherifying agent generation alkoxide, after reaction finishes through neutralization, filtration, washing, drying obtain product of the present invention with pulverizing.
Hydroxyalkyl cationic guar gum according to method for preparing can be the solid or the aqueous solution on form, can be according to user's the specific customization that requires.This solid product is the pale yellow powder shape, becomes the aqueous solution to get final product with cold water at normal-temperature dissolution during preparation, need not add preservative agent in the storage life, and viscosity does not change with the storage time, and its retention aid and filtering aid performance does not prolong with the storage time and reduces.Recommending the storage time is two weeks to month.
The hydroxyalkyl cationic guar gum of the present invention's preparation is as the paper pulp retention and drainage aid agent, its application process is: earlier hydroxyalkyl cationic guar gum is mixed with 0.5～1.5% aqueous solution, then the described hydroxyalkyl cationic guar gum aqueous solution is joined concentration and be in 0.5% the pulp suspension, other technology is with common paper technology, and the addition of described hydroxyalkyl cationic guar gum is 0.05～1.0% of a paper pulp dry pulp quality.
When above-mentioned application process was used for crushed news paper pulp, the dosage of hydroxyalkyl cationic guar gum was 0.1～0.5% of a crushed news dry pulp quality.Height according to beating degree, the addition that how much can select product of the present invention of the content of fiber fines and secondary stock anionic trash, the retention rate can be brought up to 81% under the optimal conditions from 58% of blank, and freeness drops to 28 ° of SR from 50 ° of blank SR.Therefore the use of product of the present invention improves the retention of fiber fines, improves the drainage rate of press section, can strengthen the reclamation rate of secondary stock, is beneficial to the production cost of environmental protection and reduction papermaking enterprise.
When above-mentioned application process was used for useless paper in the office paper pulp, the dosage of cation guar gum was 0.1～0.2% of the dry pulp quality of useless paper in the office, and compound method is with being used for crushed news paper pulp method.When obtaining identical retention and drainage effect, the consumption of cationic starch is 2.5%, and it is few that the hydroxyalkyl cationic guar gum of this explanation prepared of the present invention has a consumption, aquation dissolving easily, the advantage of stable performance.
When above-mentioned application process was used for useless watt of distracted paper paper pulp, the dosage of hydroxyalkyl cationic guar gum was 0.05～0.2% of useless watt distracted paper dry pulp quality, and compound method is with being used for crushed news paper pulp method.
When above-mentioned application process was used for cigarette paper paper pulp, the dosage of hydroxyalkyl cationic guar gum was 0.05～0.25% of a cigarette paper dry pulp quality, and compound method is with being used for crushed news paper pulp method.
Advantage of the present invention and effect:
The hydroxyalkyl cationic guar gum that utilizes the present invention to prepare had both had quaternary ammonium cation in the molecule, again grafting the nonionic hydroxyalkyl group.Cationic characteristic adds the relative molecular mass of appropriateness control, makes product of the present invention more can solve paper stock effectively than other retention agent and is shaped and shear problem.It has similar plants fibrocyte structure, thereby fiber is had good affinity; It can be adsorbed in fiber surface rapidly, reduce and in and the electric charge of fiber surface, make the slurry current potential close, reduce between the particle and the mutual repulsive force between the fiber, and neat solid netted bridge crosslinking structure is arranged well-balancedly and be combined into to the fiber of chaotic to equipotential.Its characteristic shows as:
1) improves drainability, be easy to increase and copy the chart speed degree, improve integral production efficient;
2) anionic impurity can be separated, improve the retention effect, improve the white-water system degree of purification;
3) help to increase press dewatering pressure, shorten and cure the time;
4) fiber there is peptizaiton, fiber is evenly distributed, improve paper strength;
5) the dye light stability energy of enhancing paper;
6) in plain boiled water, can polymerization not deposit, improve wet end stability; Reduce discharge of wastewater.
The technology of the present invention characteristics are that a step puddling synthesis technique is simple, and intermediate products needn't separation and purification, can be directly or carry out subsequent reactions simultaneously.And make full use of reaction heat in the building-up process, reduce energy consumption.Owing to use phase transfer catalyst, shorten the hydroxyalkyl etherificate reaction time greatly, shortened reaction time, improved the production capacity of product.
Ethoxy in the hydroxyalkyl cationic guar gum molecule of the present invention's preparation or hydroxypropyl are given its significant fast hydrating dissolving swelling characteristics, make it be fit to add use with the form of dry powder or slurries.It has the functional group similar to fibre structure---can reduce the paper dry linting and fall hair and show good adhesive effect; Excellent dye and filler retention performance reduce the filler loss; Reduce beating degree, especially in reclaiming paper production, can from paper pulp, separate anionic impurity, and can entangle whole and manage the long and short fiber of straight chaotic, improve wet end stability, improve every physical and chemical index of paper.
The hydroxyalkyl cationic guar gum of the present invention preparation is met water in room temperature can be dissolved into settled solution fast, compares with the modified starch chemicals, does not need the high temperature gelatinization, simple to operate, is beneficial to cut down the consumption of energy and reduce equipment investment; It is very big that product antibiont degradation capability of the present invention and former melon rubber powder are compared raising, 1% aqueous solution is constant substantially in the above viscosity of room temperature placement two weeks, retention and drainage effect is unaffected, and the starch base retention and drainage aid agent must be prepared use on the same day same day, otherwise serviceability can not get guaranteeing.
Can be according to the different component of paper pulp, the addition of beating degree and other auxiliary agents is adjusted its consumption, thus the performance synergistic function, the suitable paper kind scope of expansion product of the present invention, as: speciality paper, high-grade cigarette paper and drawing paper.
The specific embodiment
Below in conjunction with embodiment the present invention is described in further detail, but embodiments of the present invention are not limited thereto.
Embodiment 1
The not purified former powder of guar gum of 50 grams, be distributed in the mixed liquor of 80 gram industrial alcohol and 50 gram water, join in the common there-necked flask, logical nitrogen, stirring at room 10 minutes, add 10 gram sodium hydrate aqueous solutions (naoh concentration 25%) and soak alkalization 1.5 hours, drip 24 gram 3-chlorine in room temperature, the solution of 2-Hydroxyproyl Trimethyl ammonium chloride and 10.5 gram water, the dropping time is 20 minutes, be warmed up to 55 degree then, react after 3.5 hours, material is transferred in the autoclave, add hexadecyl benzyl dimethly ammonium chloride 5 grams, at inflated with nitrogen and vacuumizing under the condition, suck chlorethanol 20 grams, suck 15 gram sodium hydroxide solutions (concentration is 60%), reaction temperature is spontaneous to rise to 40 degree reactions 5 hours from room temperature, cooling is transferred pH value to 8.5 with concentrated hydrochloric acid.Material makes solvent separate with solid material through suction filtration, is dry under the 70 degree conditions with filter cake in vacuum, temperature, vacuum 0.1MPa, 8 hours drying times.To dry the back solid and be crushed to 100 orders, and make hydroxyalkyl cationic guar gum at last, weight is 80 grams.After testing, this product nitrogen content 1.32%, nonionic substitution value (MS) is 0.5.
Embodiment 2
The not purified former powder of guar gum of 50 grams, be distributed in the mixed liquor of 400 gram isopropyl alcohols and 40 gram water, join in the there-necked flask after the mixing of materials, logical nitrogen, stirring at room 10 minutes, add 50 gram potassium hydroxide aqueous solutions (concentration of potassium hydroxide 10%) and soak alkalization 0.5 hour, drip the solution of 10 gram epoxypropyl trimethylammonium chloride amine and 10 gram water in room temperature, the dropping time is 20 minutes, be warmed up to 60 degree then, react after 3.0 hours, material is transferred in the autoclave, add hexadecyl benzyl dimethly ammonium chloride 5 grams, inflated with nitrogen and vacuumizing under the condition sucks expoxy propane 10 grams, and reaction temperature is spontaneous to rise to 50 degree reactions 1.5 hours from room temperature, cool to 35 degree subsequently, transfer pH value to 8.2 with acetic acid.Material makes solvent separate with solid material through suction filtration, send vacuumize with filter cake, baking temperature 70 degree, vacuum 0.1MPa, 8 hours drying times.To dry the back solid and be crushed to 100 orders, and make hydroxyalkyl cationic guar gum at last, weight is 85 grams.After testing, this product nitrogen content 0.50%, nonionic substitution value (MS) is 0.5.
Embodiment 3
The not purified former powder of guar gum of 50 grams, be distributed in the mixed liquor of the 60 gram tert-butyl alcohols and 60 gram water, join in the there-necked flask after the mixing of materials, logical nitrogen, stirring at room 10 minutes, add 30 gram potassium hydroxide solutions (concentration of potassium hydroxide 25%), in soaking at room temperature alkalization 45 minutes, drip 30 gram self-control 3-chloro-2-hydroxypropyl pyridine hydrochlorides (light yellow transparent solution, valid density 70%), the dropping time is 20 minutes, under the temperature of 35 degree, react after 6 hours then, material is transferred in the autoclave, add hexadecyl benzyl dimethly ammonium chloride 5.0 grams, inflated with nitrogen and vacuumizing under the condition sucks expoxy propane 50 grams, and reaction temperature is spontaneous to rise to 60 degree reactions 4 hours from room temperature, cooling is transferred pH value to 7.8 with citric acid.Material makes solvent separate with solid material through suction filtration, and filter cake is dissolved in 1.5 premium on currency, stirs 0.5 hour on magnetic stirring apparatus, obtains the 5% transparent thickness aqueous solution.With a part of filter cake with ethanol/water mixed solution (alcohol/water ratio is 1: 1) washed twice after, make hydroxyalkyl cationic guar gum at last, after testing, its nitrogen content 2.52%, nonionic substitution value (MS) is 2.5.
Embodiment 4
The former powder of 50 gram guar gums, be dispersed in the mixed liquor of 80 gram absolute ethyl alcohols and 20 gram water, at room temperature directly add 30 gram caustic alcohols (concentration is 100%), inflated with nitrogen, in autoclave, soak alkalization 1 hour, suck the 50 gram self-control 3-chloro-2-hydroxypropyl pyridine hydrochloride aqueous solution (valid density 50%) and 25 gram chlorethanols, stirring at room 1 hour, pump into 25 gram sodium hydroxide solutions (naoh concentration 60%) then, temperature reaction, 50 degree reactions 1 hour, continue to be warmed up to 75 degree, reacted 3 hours.Product is transferred about PH to 7 with glacial acetic acid after lowering the temperature naturally, and press filtration separates organic solvent, and filter cake is ground into 100 order powder after the oven dry of normal pressure hot air drier, make hydroxyalkyl cationic guar gum at last.After testing, hydroxyalkyl cationic guar gum nitrogen content 1.55%, nonionic molar substitution 0.91.
Embodiment 5
The former powder of 50 gram guar gums, be dispersed in the mixed liquor of 100 gram absolute methanols and 20 gram water, at room temperature add the sodium hydrate aqueous solution of 10 gram sodium methoxides and 10 gram concentration 25%, inflated with nitrogen, alkalization is 1.0 hours in autoclave, suck 50 gram self-control 3-chloro-2-hydroxypropyl quinoline hydrochlorides, the dropping time is 20 minutes, is warmed up to 75 degree then, react after 2.5 hours, material is transferred in the autoclave, added hexadecyl benzyl dimethly ammonium chloride 5.0 grams, inflated with nitrogen and vacuumizing under the condition, suck oxirane 50 grams, reaction temperature rises to 75 degree reactions 1 hour from room temperature, and cooling is transferred pH value to 7.5 with boric acid.Material makes solvent separate with solid material through suction filtration, and filter cake is ground into 100 order powder after the oven dry of normal pressure hot air drier, make hydroxyalkyl cationic guar gum at last.After testing, the hydroxyalkyl cationic guar gum nitrogen content 2.12% that present embodiment makes, nonionic molar substitution 3.52.
Embodiment 6
The hydroxyalkyl cationic guar gum of example 1 preparation is mixed with 0.5% aqueous solution, the hydroxyalkyl cationic guar gum aqueous solution according to 0.1～1.0% (accounting for paper pulp dry pulp weight with the hydroxyalkyl cationic guar gum powder calculates) consumption is added in the crushed news mass suspension of concentration 0.5%, and other technology is with common paper technology.
Utilize DDJ dynamic drainage analyzer to survey its retention performance, and measure freeness simultaneously.
Used laboratory apparatus:
Conductivity gauge; The PH meter; Schooper-Riegler beating degree tester; Dynamic drainage analyzer (DDJ); 2100P type nephelometer.DDJ dynamic drainage analyzer and nephelometer are used.
Step: it is 0.5% suspension that 2 gram oven dry stocks are mixed with concentration, filter screen is with 200 order nets, measure 500 milliliters in the DDJ instrument, add the product aqueous solution of the present invention, the rotating speed with 750rpm stirs simultaneously, use manual time-keeping, open the liquid valve immediately after stirring for 10 seconds, access and stop after the 100ml filtrate stirring, on nephelometer, measure its light transmittance with this 100ml filtrate, be scaled filter liquor concentration (being machine water concentration), calculate the initial journey retention according to filter liquor concentration and paper stock concentration then.The initial journey retention is meant that slurry stays the percentage of total solid in solid content on the page and the slurry by papermaking wire-cloth.Computing formula is: initial journey retention (FPR)=(1-filter liquor concentration/sample solution concentration) * 100%.Experimental data sees Table 1.
Process conditions: PH7.0, electrical conductivity 2000us/cm, 750 rev/mins of rotating speeds.
The result is as shown in table 1.
Experimentation shows: hydroxyalkyl cationic guar gum is added to secondary stock suspension system with 0.1%～1.0% (accounting for paper pulp dry pulp weight with the hydroxyalkyl cationic guar gum powder calculates) consumption, will be by charging neutrality, the strong effect of adsorption bridging and hydrogen promotes keeping of fiber fines, machine water concentration is reduced, freeness obviously descends, and reduces beating energy consumption, is beneficial to the paper industry white water loop and uses, be beneficial to and alleviate the pollution of paper industry, thereby embodied outstanding retention aid and filtering aid performance environment.
The crushed news slurry initial journey retention and the freeness information slip of the different hydroxyalkyl cationic guar gum additions of table 1
| Dosage (%) | Initial journey retention (%) | Freeness (° SR) |
| 0 | 58 | 50 |
| 0.1 | 70 | 38 |
| 0.2 | 75 | 35 |
| 0.3 | 78 | 32 |
| 0.4 | 80 | 30 |
| 0.5 | 81 | 28 |
| 1.0 | 75 | 32 |
Table 1 shows: product of the present invention is 0.1% o'clock at dosage, and the retention of fiber and fiber fines has improved 20.6%, later on along with consumption increases, retention slowly improves, when consumption was 0.5%, the retention rate reached 81%, and Kong Bai retention has improved 39.7% relatively.When further increasing retention, consumption descends on the contrary.
Embodiment 7
The product of example 1 preparation is mixed with 0.5% aqueous solution, consumption (accounting for paper pulp dry pulp weight with the cation guar gum powder calculates) according to the hydroxyalkyl cationic guar gum of table 2 is added in the useless chancery paper mass suspension of concentration 0.5%, and other technology is with common paper technology.Utilize DDJ dynamic drainage analyzer to survey its retention performance, and measure freeness simultaneously.Experimental implementation step and process conditions are with example 6.Experimental data sees Table 2.
The useless office paper pulp initial journey retention and the freeness information slip of the different hydroxyalkyl cationic guar gum additions of table 2
| Dosage (%) | Initial journey retention (%) | Freeness (° SR) |
| 0 | 67 | 41 |
| 0.08 | 72 | 35 |
| 0.1 | 78 | 32 |
| 0.15 | 82 | 30 |
| 0.2 | 86 | 29 |
Table 2 shows: along with the increase of hydroxyalkyl cationic guar gum addition, beating degree also obviously descends thereupon, and the initial journey retention improves.
Embodiment 8
The product of example 1 preparation is mixed with 0.5% aqueous solution, be added to according to table 3 consumption (accounting for paper pulp dry pulp weight with the cation guar gum powder calculates) in 0.5% the useless corrugated paper mass suspension, utilize DDJ dynamic drainage analyzer to survey its retention performance, and measure freeness simultaneously.Experimental implementation step and process conditions are with example 6.Experimental data sees Table 3.
Table 3 shows: along with the increase of hydroxyalkyl cationic guar gum addition, beating degree also obviously descends thereupon, and the initial journey retention improves.Addition was at 0.15% o'clock, and useless corrugation paper pulp beating degree drops to 32 ° of SR from 48 ° of SR that do not add hydroxyalkyl cationic guar gum.
The useless corrugation paper pulp initial journey retention and the freeness information slip of the different hydroxyalkyl cationic guar gum additions of table 3
| Dosage (%) | Initial journey retention (%) | Freeness (° SR) |
| 0 | 62 | 48 |
| 0.05 | 71 | 40 |
| 0.1 | 79 | 35 |
| 0.15 | 81 | 32 |
| 0.2 | 83 | 29 |
Embodiment 9
The product of example 5 preparations is mixed with 0.5% aqueous solution, consumption according to 0.05%-0.25% hydroxyalkyl cationic guar gum melon glue (accounting for paper pulp dry pulp weight with the cation guar gum powder calculates) is added in the cigarette paper pulp suspension of concentration 0.5%, utilize DDJ dynamic drainage analyzer to survey its retention performance, and measure freeness simultaneously.Laboratory apparatus and process conditions are with example 6.Experimental data sees Table 4.
The cigarette paper paper pulp initial journey retention and the freeness information slip of the different hydroxyalkyl cationic guar gum additions of table 4
| Dosage (%) | Initial journey retention (%) | Freeness (° SR) |
| 0 | 46.9 | 81 |
| 0.05 | 70 | 75 |
| 0.1 | 75 | 70 |
| 0.15 | 82 | 65 |
| 0.20 | 82 | 62 |
| 0.25 | 80 | 63 |
As can be seen from Table 4, along with the increase of product addition of the present invention, beating degree also obviously descends thereupon, and the initial journey retention improves.Addition brought up to 82% to the retention of fiber and fiber fines from 46.9% of blank at 0.15% o'clock.Addition was at 0.25% o'clock, and the initial journey retention descends on the contrary to some extent, and freeness and dosage are that variation in 0.15% o'clock is not obvious.
Embodiment 6～9 shows, can keep fiber preferably and improve drainage when hydroxyalkyl cationic guar gum is used as retention and drainage aid agent, and a comparatively suitable amount ranges is arranged.Concrete consumption depends on the kind of secondary stock, fines content, anionic trash content etc.Therefore must decide according to the retention aid and filtering aid experimental result, optimum amount scope provided by the invention only plays directive function.
Claims (4)
1, one-step slurry preparation method of hydroxylalkyl cationic guar gum is characterized in that comprising the steps and process conditions:
(1) guar gum soaks alkalization, in mass fraction, 100 parts of former powder of not purified guar gum are joined in 200～880 parts of alcohol/aqueous mixtures, filling under the nitrogen condition, adding 20～100 parts of the aqueous solution of concentration 10～100% base catalysts subsequently, soaking alkalization 0.5～1.5h, make alkalization guar gum suspension, the alcohol of described alcohol/aqueous mixtures is 1～10: 1 with the quality ratio, and described alcohol is methyl alcohol, absolute ethyl alcohol, industrial alcohol, isopropyl alcohol or the tert-butyl alcohol;
(2) guar gum cation graft reaction, in mass fraction, be that 50～70% cationic etherifying agent aqueous solution join in the alkalization guar gum suspension of step (1) gained with 10～100 parts of concentration, be under 35～75 degree conditions in temperature, reacted 2～6 hours, and made cationic intermediates;
(3) guar gum hydroxyalkylation reaction, in mass fraction, 0～10 portion of phase transfer catalyst is joined in the cationic intermediates of step (2) gained, fill nitrogen, vacuumize and-0.1～0.1MPa pressure condition under, add 20～100 portions of alkoxyl etherifying agents, replenish 0～25 part of 60% sodium hydroxide solution, exothermic heat of reaction makes spontaneous 40～75 degree that are raised to of temperature of charge, reacted 1～5 hour, cool to room temperature subsequently, and regulate material pH value to 7.0～8.5 with acidic materials, make with the mud state and be dispersed in hydroxyalkylation cation guar gum in alcohol/aqueous solution;
(4) step (3) the muddy attitude that is able to is dispersed in alcohol/aqueous solution the hydroxyalkylation cation guar gum after filtration, washing, dry, pulverize after, make hydroxyalkyl cationic guar gum.
2,, it is characterized in that the alcohol of alcohol/aqueous mixtures in the described step (1) is 1.2～9: 1 with the quality ratio according to the described method of claim 1; Described base catalyst is a NaOH, potassium hydroxide, sodium methoxide, a kind of and more than one mixtures in the caustic alcohol.
3, according to the described method of claim 1, it is characterized in that described step (2) reaction temperature is 45～70 degree, the reaction time is 2.5～5 hours, and described cationic etherifying agent is a 3-chloro-2-Hydroxyproyl Trimethyl ammonium chloride, arsenic thiamine hydrochloride, quinoline hydrochloride or epoxypropyl trimethylammonium chloride amine.
4, according to the described method of claim 1, it is characterized in that the reaction time is 1.5～4.0 hours in the described step (3), described phase transfer catalyst is a hexadecyl benzyl dimethly ammonium chloride; Described alkoxyl etherifying agent is oxirane, expoxy propane, epoxy butane or chlorethanol or 2-chloropropyl alcohol; Described acidic materials are hydrochloric acid ,] acetic acid, boric acid, citric acid.
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| CN101210401B (en) * | 2007-12-24 | 2010-06-02 | 上海东升新材料有限公司 | Modified guar surface sizing agent and its preparing method and application |
| CN101210055B (en) * | 2007-12-24 | 2011-08-31 | 上海东升新材料有限公司 | Modified guar gum, preparing method thereof, and application of the same in preparing tobacco thin sheet |
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