CN100591695C - Polyanion cellulose preparation method - Google Patents
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Abstract
The present invention discloses polyanionic cellulose with a special quality, the multi-step slurry process for preparing the polyanionic cellulose and the ternary complex solvent required. The complex solvent is composed of (A) from 71 percent to 87 percent by weight of isopropyl alcohol, (B) from 10 percent to 20 percent by weight of alcohol and from 71 percent to 87 percent by weight of the soft water. The multi-step slurry process for preparing the polyanionic cellulose has a more excellent technical effect on material economizing, time saving and the properties of product than the traditional one-step slurry process for preparing the polyanionic cellulose. Compared with the properties the product produced by the traditional method, the acid resistance is raised by more than 20 percent, and the viscosity is greatly improved. The polyanionic cellulose is widely used in the fields like petroleum, paint, detergent, building materials, textile industry, paper marking, medicines, foodstuff, etc.
Description
Technical field
The invention belongs to field of fine chemical, especially the ternary double solvents of Polyanionic Cellulose (PAC), prepare the Polyanionic Cellulose of the multistep slurry process of Polyanionic Cellulose and the preparation of this method and in the application in fields such as oil, coating, washing composition, building materials, weaving, papermaking, medicine, food with this solvent.
Background technology
The cellulose-derived product industry of China is started in eighties of last century sixties, the developing history surplus in the of existing 40 year so far, and wherein carboxymethyl cellulose (CMC) is long, the most largest cellulose-derived product of domestic production time.With abroad compare, the quantity of China ether of cellulose manufacturing enterprise is too much, throughput is greater than demand, scope of the enterprise and difference of technology level are bigger, lack the scientific research input, the Product Renewal progress is slow.Along with developing rapidly of fine chemistry industry industry, people require more and more higher to aspects such as the quality of ether of cellulose, kind, specifications.The plain product of conventional fibre is single because of its water-soluble effect at present, and application is restricted, and demand also constantly descends, and powdery polyanionic cellulose with high degree of substitution demand just grows steadily.The Polyanionic Cellulose product, because its molecular weight distribution is more concentrated, substituted radical distributes more even, salt tolerance and anti-dehydration ability with comparison brilliance, can effectively control fluidic and run off, be applied to ocean or continental rise drilling well, in drilling fluid as fluid loss agent or thickening material.It also is widely used in industries such as coating, food, building materials, washing composition, weaving, papermaking, medicine, chemical industry.Polyanionic Cellulose is similar to CMC on molecular structure, but is better than CMC on the performance, and it is the upgraded product of CMC thus.There are a lot of shortcomings in the preparation technology of Polyanionic Cellulose on the current social, and particularly these shortcomings mainly show the following aspects:
What 1, the alkalinization step in the traditional processing technology was commonly used is this single solvent of ethanol, single solvent---ethanol has significant disadvantages in use in the alkalization process, through the product that series reaction obtained, particle is bigger than normal, inhomogeneous again, performance index instabilities such as substitution value wherein, viscosity, alkalization process are not thorough, imperfection, have influenced the result of use of product.
2, alkali is put into single solvent---in the ethanol, dissolution rate is very slow, and it is also inhomogeneous to distribute, after causing dropping into purified cotton, have a strong impact on the alkalization effect, influence the etherificate effect then, the requirement that finally makes salt tolerance, the acid resistance of product not reach the application performance index.
3, traditional " a step slurry process " adopts that kneader will alkalize, material carries out hybrid reaction by stirring after the etherificate.Under this state, local reaction takes place very easily, etherificate is not thorough, causes the substitution value of product inhomogeneous, and production efficiency is low.
Summary of the invention
In order to overcome the deficiencies in the prior art, the contriver is on the basis of a large amount of experiments, discovery is on the preparation technology's of traditional Polyanionic Cellulose basis, it is not thorough to utilize " ternary double solvents " employing " multistep slurry process " can overcome the alkalization etherificate, product performance index is nonconforming, the technical barrier that production efficiency is low.The contriver has produced the Polyanionic Cellulose that possesses special trait by this novel preparation technology, use and test through too much tame unit, verify that this product can be applied in the fields such as petroleum industry, coating, washing composition, building materials, weaving, papermaking, medicine, food.
One of purpose of the present invention is: a kind of Polyanionic Cellulose that possesses special trait is provided.
Two of purpose of the present invention is: a kind of ternary double solvents that is used to prepare Polyanionic Cellulose is provided.
Three of purpose of the present invention is: this preparation method who possesses the Polyanionic Cellulose of special trait is provided.
Polyanionic Cellulose of the present invention possesses the feature of general formula (I):
(I)
R=H in the formula, or-CH
2-COONa
Polymerization degree n=200～3000
The ternary double solvents that is used to prepare above-mentioned Polyanionic Cellulose is made up of following component:
A, Virahol 71%-87%
B, ethanol 10%-20%
C, soft water 3%-9%
Above-mentioned ternary double solvents, more preferably the component selection is:
A, Virahol 78%
B, ethanol 14%
C, soft water 8%
A kind of multistep slurry process for preparing Polyanionic Cellulose comprises the steps:
(1) in three reactors, injects ternary double solvents 1.8-2.2 ton respectively;
(2) No. 1 reactor is warming up to 20 ℃-25 ℃, vacuumizes, open clean-out cover, drop into sheet alkali 460-480kg, be warming up to 70 ℃-75 ℃ earlier, 52 ℃ of-58 ℃ of constant temperature, continuously stirring 90-120 minute;
(3) No. 2 reactors are warming up to 70 ℃-75 ℃, are cooled to 15 ℃-22 ℃ then, vacuumize, open clean-out cover, drop into purified cotton 540-560kg, 22 ℃ of-30 ℃ of following constant temperature, continuously stirring 80-120 minute;
(4) drop into Mono Chloro Acetic Acid 440-460kg to No. 3 reactors, 30 ℃ of-40 ℃ of constant temperature, continuously stirring 180-220 minute;
(5) No. 1 reactor is vacuumized, after the purified cotton powder in No. 2 reactors stuck with paste through being forced into 4mpa inject in No. 1 reactor, the back adds nitrogen to 2mpa, 3 times repeatedly, 30 ℃ of-40 ℃ of constant temperature, continuously stirring 90-120 minute;
(6) No. 1 reactor is vacuumized, after the Mono Chloro Acetic Acid in No. 3 reactors be forced into 4mpa inject in No. 1 reactor, the back adds nitrogen to 2mpa, 4 times repeatedly, 35 ℃ of-40 ℃ of constant temperature, continuously stirring 120-130 minute;
(7) No. 1 reactor is vacuumized, the back adds acetic acid 28-35kg, in and 30-50 minute, measuring the pH value is 6.5～8, gets final product discharging.
The multistep slurry process of above-mentioned preparation Polyanionic Cellulose, optimal scheme are to carry out following steps:
(1) in three reactors, injects 2 tons of ternary double solventss respectively;
(2) No. 1 reactor is warming up to 22 ℃, vacuumizes, open clean-out cover, drop into sheet alkali 475kg, be warming up to 72 ℃ earlier, at 55 ℃ of constant temperature, continuously stirring 100 minutes;
(3) No. 2 reactors are warming up to 72 ℃, are cooled to 18 ℃ then, vacuumize, open clean-out cover, drop into purified cotton 550kg, at 25 ℃ of following constant temperature, continuously stirring 100 minutes;
(4) drop into Mono Chloro Acetic Acid 450kg to No. 3 reactors, at 35 ℃ of constant temperature, continuously stirring 200 minutes;
(5) No. 1 reactor is vacuumized, after the purified cotton powder in No. 2 reactors stuck with paste through being forced into 4mpa inject in No. 1 reactor, the back adds nitrogen to 2mpa, 3 times repeatedly, at 35 ℃ of constant temperature, continuously stirring 100 minutes;
(6) No. 1 reactor is vacuumized, after the Mono Chloro Acetic Acid in No. 3 reactors be forced into 4mpa inject in No. 1 reactor, the back adds nitrogen to 2mpa, 4 times repeatedly, at 36 ℃ of constant temperature, continuously stirring 125 minutes;
(7) No. 1 reactor is vacuumized, the back adds acetic acid 30kg, in and 40 minutes, measuring the pH value is 7, gets final product discharging.
If the purified cotton that the multistep slurry process of aforementioned preparation Polyanionic Cellulose is adopted is pulverized after handling through opener again, guarantee its loose density 〉=120g/l (being certain volumetrical grammes per square metre), effect can be more superior.This method adopts Virahol, ethanol and soft " ternary double solvents ", make alkalization more thorough, perfect, the reaction degree of uniformity is significantly increased, the performance of the product that obtains is compared with traditional product that production method obtains, acid resistance improves more than 20%, and salt tolerance improves more than 30%.This method has adopted " multistep slurry process ", choline still, etherificate still have been increased, and connect totally-enclosed DCS electronic system, utilize three reactors material to be carried out the cascade reaction and the upgrading reaction of different steps, it is even more, thorough that material is reacted to each other, and shorten time difference of each step of reaction, improved material reaction speed.Compare and saved non-cutting time with " a step slurry process " production technique, realized the continuous production in the part technology, production efficiency has improved more than 20%.
The Polyanionic Cellulose of producing by technical solution of the present invention has passed through test, detection, evaluation and on probation, the result proves that this kind Polyanionic Cellulose has special superior quality, measures it by nuclear magnetic resonance technique and possesses performance and the constitutional features that is different from product that traditional method obtains.And this technical matters is advanced rationally, coordinative composition of equipments adaptation, stable operation, production process do not have " three wastes " discharging substantially.The anti-salt of product, water retention property are superior, can be widely used in the fields such as petroleum industry, coating, washing composition, building materials, weaving, papermaking, medicine, food.Society's reflection is good, has remarkable economical, social benefit.
Description of drawings
Fig. 1 is the typical process block diagram of technical solution of the present invention.
Fig. 2 is the Polyanionic Cellulose nmr analysis graphic representation with the traditional method preparation.
Fig. 3 is the Polyanionic Cellulose nmr analysis graphic representation with the inventive method preparation.
Embodiment
Specify technology contents of the present invention and effect below in conjunction with embodiment, comparative experiments example and accompanying drawing:
Embodiment 1
Following component is mixed, and preparation is used to prepare the ternary double solvents of Polyanionic Cellulose: A, Virahol (concentration 〉=98%), 87%; B, ethanol (concentration 〉=95%), 10%; C, soft water (hardness≤3), 3%.
Embodiment 2
Following component is mixed, and preparation is used to prepare the ternary double solvents of Polyanionic Cellulose: A, Virahol, 71%; B, ethanol, 20%; C, soft water, 9%.
Embodiment 3
Following component is mixed, and preparation is used to prepare the ternary double solvents of Polyanionic Cellulose: A, Virahol, 78%; B, ethanol, 14%; C, soft water, 8%.
Embodiment 4
Following component is mixed, and preparation is used to prepare the ternary double solvents of Polyanionic Cellulose: A, Virahol, 76%; B, ethanol, 18%; C, soft water, 6%.
Embodiment 5
Carry out the preparation that following step is carried out Polyanionic Cellulose successively:
(1) in three reactors, injects 1.8 tons of ternary double solventss respectively;
(2) No. 1 reactor is warming up to 20 ℃, vacuumizes, (why being called " manhole plate ", is to pass through because this lid mouth can hold a people to open manhole plate, for ease of understanding, also can be called " clean-out cover "), drop into sheet alkali 460kg, be warming up to 70 ℃, 52 ℃ of constant temperature, continuously stirring 90 minutes;
(3) No. 2 reactors are warming up to 70 ℃, are cooled to 15 ℃ then, vacuumize, open clean-out cover, drop into purified cotton 540kg, constant temperature is at 22 ℃, continuously stirring 80 minutes;
(4) dropping into concentration to No. 3 reactors is 96.5% Mono Chloro Acetic Acid 440kg, 30 ℃ of constant temperature, continuously stirring 180 minutes;
(5) No. 1 reactor is vacuumized after, the purified cotton powder of the liquid state in No. 2 reactors is stuck with paste through pressurization (pressure is 4mpa), inject in No. 1 reactor, after finishing, add nitrogen to 2mpa, (promptly add nitrogen to 2mpa, be evacuated to-2mpa for 3 times repeatedly; Add nitrogen again to 2mpa, be evacuated to-2mpa; Successively repeatedly, its objective is and avoid other gases participation reactions in the still), 30 ℃ of constant temperature, continuously stirring 90 minutes;
(6) No. 1 reactor is vacuumized, after the Mono Chloro Acetic Acid in No. 3 reactors be forced into 4mpa inject in No. 1 reactor, the back adds nitrogen to 2mpa, 4 times repeatedly, at 35 ℃ of constant temperature, continuously stirring 120 minutes;
(7) No. 1 reactor is vacuumized, adds concentration then and be 99% acetic acid 28kg, in and after 30 minutes, measuring the pH value is 6.5, it is qualified to be, discharging.
Embodiment 6
Carry out the preparation that following step is carried out Polyanionic Cellulose successively:
(1) in three reactors, injects 2.2 tons of ternary double solventss respectively;
(2) No. 1 reactor is warming up to 25 ℃, vacuumizes, open clean-out cover, drop into 480 tons in sheet alkali, be warming up to 75 ℃, 58 ℃ of constant temperature, continuously stirring 120 minutes;
(3) No. 2 reactors are warming up to 75 ℃, are cooled to 22 ℃ then, vacuumize, open clean-out cover, drop into purified cotton 560kg, constant temperature is at 30 ℃, continuously stirring 120 minutes;
(4) drop into Mono Chloro Acetic Acid 460kg, continuously stirring 220 minutes to No. 3 reactors;
(5) No. 1 reactor is vacuumized after, the purified cotton powder of the liquid state in No. 2 reactors is stuck with paste through pressurization (pressure is 4mpa), injects in No. 1 reactor, after finishing, adding nitrogen is to 2mpa, 3 times repeatedly, 40 ℃ of constant temperature, continuously stirring 120 minutes;
(6) No. 1 reactor is vacuumized, after the Mono Chloro Acetic Acid in No. 3 reactors be forced into 4mpa inject in No. 1 reactor, the back adds nitrogen to 2mpa, 4 times repeatedly, at 40 ℃ of constant temperature, continuously stirring 130 minutes;
(7) No. 1 reactor is vacuumized, adds acetic acid 35kg then, in and 50 minutes, measuring the pH value is 8, it is qualified to be, discharging.
Embodiment 7
Carry out the preparation that following step is carried out Polyanionic Cellulose successively:
(1) in three reactors, injects 2 tons of ternary double solventss respectively;
(2) No. 1 reactor is warming up to 22 ℃, vacuumizes, open clean-out cover, drop into sheet alkali 475kg, be warming up to 72 ℃ earlier, at 55 ℃ of constant temperature, continuously stirring 100 minutes;
(3) No. 2 reactors are warming up to 72 ℃, are cooled to 18 ℃ then, vacuumize, open clean-out cover, drop into purified cotton 550kg, at 25 ℃ of following constant temperature, continuously stirring 100 minutes;
(4) drop into Mono Chloro Acetic Acid 450kg to No. 3 reactors, at 35 ℃ of constant temperature, continuously stirring 200 minutes;
(5) No. 1 reactor is vacuumized, after the purified cotton powder in No. 2 reactors stuck with paste through being forced into 4mpa inject in No. 1 reactor, the back adds nitrogen to 2mpa, 3 times repeatedly, at 35 ℃ of constant temperature, continuously stirring 100 minutes;
(6) No. 1 reactor is vacuumized, after the Mono Chloro Acetic Acid in No. 3 reactors be forced into 4mpa inject in No. 1 reactor, the back adds nitrogen to 2mpa, 4 times repeatedly, at 36 ℃ of constant temperature, continuously stirring 125 minutes;
(7) No. 1 reactor is vacuumized, the back adds acetic acid 30kg, in and 40 minutes, measuring the pH value is 7, gets final product discharging.
Embodiment 8
Carry out the preparation that following step is carried out Polyanionic Cellulose successively:
(1) in three reactors, injects 2 tons of ternary double solventss respectively;
(2) No. 1 reactor is warming up to 24 ℃, vacuumizes, open manhole plate, drop into sheet alkali 458kg, be warming up to 74 ℃, 56.5 ℃ of constant temperature, continuously stirring 105 minutes;
(3) No. 2 reactors are warming up to 75 ℃, are cooled to 21 ℃ then, vacuumize, open manhole plate, drop into purified cotton 540kg, purified cotton is pulverized, the loose density that makes purified cotton is greater than 120g/l, guaranteeing purified cotton homogeneous reaction in solvent, constant temperature is at 28 ℃, continuously stirring 85 minutes;
(4) drop into Mono Chloro Acetic Acid 430kg, 38 ℃ of constant temperature, continuously stirring 205 minutes to No. 3 reactors;
(5) No. 1 reactor is vacuumized after, the purified cotton powder of the liquid state in No. 2 reactors is stuck with paste through pressurization (pressure is 4mpa), inject in No. 1 reactor, after finishing, adding rare gas element---nitrogen is to 2mpa, (promptly adds nitrogen to 2mpa, is evacuated to-2mpa for 3 times repeatedly; Add nitrogen again to 2mpa, be evacuated to-2mpa; In proper order repeatedly, its objective is and avoid other gases participation reactions in the still), 38 ℃ of constant temperature, continuously stirring 92 minutes;
(6) No. 1 reactor is vacuumized, after the Mono Chloro Acetic Acid in No. 3 reactors be forced into 4mpa inject in No. 1 reactor, the back adds nitrogen to 2mpa, 4 times repeatedly, at 36 ℃ of constant temperature, continuously stirring 125 minutes;
(7) No. 1 reactor is vacuumized, the back adds acetic acid 32kg, in and 40 minutes, measuring the pH value is 7.5, gets final product discharging.
Comparison test example 1
The contriver adopt Polyanionic Cellulose that " ternary double solvents " and " multistep slurry process " preparation Polyanionic Cellulose and traditional " monobasic solvent " and " a step slurry process " prepare at the saving material, save time, product performance raising and the aspect such as raise the efficiency and obtained excellent technique effect, the performance of the product that obtains is compared with traditional product that production method obtains, acid resistance improves more than 20%, salt tolerance improves more than 30%, and production efficiency has improved more than 20%.Viscosity also improves a lot, referring to table one
Table one:
The technical indicator of product relatively
Comparison test example 2
The contriver utilizes
1The H-NMR nuclear magnetic resonance technique has further been analyzed the Polyanionic Cellulose difference structurally that Polyanionic Cellulose of the present invention and traditional method are obtained.Sample adopts D
2SO
4-D
2O handles, and uses acetic acid as interior mark.The results are shown in Figure 2, Fig. 3 and table two.
Table two:
Polyanionic Cellulose product of the present invention and existing procucts index are relatively
| Project | C1α-S | C1α-U | C1β-S | C2 | C3 | C6 | The proton peak area | C2∶C3∶C6 |
| Novel process | 1.0000 | 0.7044 | 0.7551 | 4.7786 | 2.4240 | 3.8121 | 21.2486 | 1.97∶1∶1.57 |
| Traditional technology | 1.0000 | 1.5623 | 0.9728 | 8.5084 | 3.7919 | 6.3931 | 51.7996 | 194∶1∶1.60 |
Area ratio according to each peak of C2, C3, C6 can calculate substituent distribution.Find out that from the result of Fig. 1 and Fig. 2 both peaking displacement study values are basic identical, difference is the peak area difference.Wherein S, U refer to the C2 that closes on C1 respectively and go up hydroxyl and be substituted and be not substituted.This shows on the product P AC molecule of the present invention-being distributed in of replacing of CH2COONa is more even than traditional product to a certain extent.
The Polyanionic Cellulose that the present invention obtained has carried out technology for detection, technical evaluation and product beta test under confidential state, the result is as follows:
1, technology for detection unit, time and conclusion:
A) detect unit: petroleum industry oilfield chemistry agent quality supervision and test center
Detection time: on March 20th, 2005; Detect conclusion: qualified.
B) detect unit: institute of drilling mud company of Shengli Petroleum Administration Bureau
Detection time: on August 2nd, 2004; Detect conclusion: qualified.
C) detect unit: Liaohe Petroleum Exploration Bureau product quality inspection station
Detection time: on July 2nd, 2004; Detect conclusion: qualified.
2, technical evaluation unit, time and conclusion:
Identify unit: Shandong Province science and technology bureau
Qualification time: on December 11st, 2004
Conclusion:
A) technical information that provides is complete complete, and data accurately, reliably meet the evaluation requirement.
B) this project is a main raw material with purified cotton, NaOH, Mono Chloro Acetic Acid etc., makes through steps such as alkalization, etherificate, washing, separation, drying, pulverizing.Technology is advanced rationally, coordinative composition of equipments adaptation, stable operation, production process do not have " three wastes " discharging substantially." the ternary double solvents " that this technology adopted, " multistep slurry ", special reaction equipment, totally-enclosed DCS Controlling System have novelty.
C) detect through Liaohe Petroleum Exploration Bureau product quality inspection station, on probation, functional, every quality index all meets the specified requirement of company standard Q/09FYT001-2004.Detection means is complete, quality assurance system is sound, can satisfy the production quality control requirement.
D) this product extensively can be used for oil, coating, washing composition, building materials, weaving, papermaking, medicine and other fields.Extensive market, the said firm has built up 2000 tons/year production equipment.
E) conscientiously discuss through the expert statement council, agree unanimously by this project technical products and identify.
3, unit on probation and suggestion:
A) unit on probation: Zhongyuan Petroleum Exploration Bureau
Time on probation: in April, 2004～2004 year November
Evaluation product: Polyanionic Cellulose (PAC-LV; PAC-HV)
Conclusion on probation: compare with external like product and to have viscosity stability preferably, heat-resisting property and anti-salt, contamination resistance are superior, and water retention property is outstanding, fully alternative similar imported product.
B) unit on probation: Chinese Liaohe Oil Field
Time on probation: December 2004 March in 2004
Evaluation product: Polyanionic Cellulose (PAC-LV; PAC-HV)
Conclusion on probation: through my company this product on probation, through comparing with external like product, anti-salt, water retention property are superior, can be used as the new-type mortar treatment agent fully.
Claims (4)
1, a kind of multistep slurry process for preparing Polyanionic Cellulose is characterized in that, comprises the steps:
(1) inject ternary double solvents 1.8-2.2 ton respectively in three reactors, described ternary double solvents is made up of following component: A, Virahol 71%-87%, B, ethanol 10%-20%, C, soft water 3%-9%;
(2) No. 1 reactor is warming up to 20 ℃-25 ℃, vacuumizes, open clean-out cover, drop into sheet alkali 460-480kg, be warming up to 70 ℃-75 ℃ earlier, 52 ℃ of-58 ℃ of constant temperature, continuously stirring 90-120 minute;
(3) No. 2 reactors are warming up to 70 ℃-75 ℃, are cooled to 15 ℃-22 ℃ then, vacuumize, open clean-out cover, drop into purified cotton 540-560kg, 22 ℃ of-30 ℃ of following constant temperature, continuously stirring 80-120 minute;
(4) drop into Mono Chloro Acetic Acid 440-460kg to No. 3 reactors, 30 ℃ of-40 ℃ of constant temperature, continuously stirring 180-220 minute;
(5) No. 1 reactor is vacuumized, after the purified cotton powder in No. 2 reactors stuck with paste through being forced into 4mpa inject in No. 1 reactor, the back adds nitrogen to 2mpa, 3 times repeatedly, 30 ℃ of-40 ℃ of constant temperature, continuously stirring 90-120 minute;
(6) No. 1 reactor is vacuumized, after the Mono Chloro Acetic Acid in No. 3 reactors be forced into 4mpa inject in No. 1 reactor, the back adds nitrogen to 2mpa, 4 times repeatedly, 35 ℃ of-40 ℃ of constant temperature, continuously stirring 120-130 minute;
(7) No. 1 reactor is vacuumized, the back adds acetic acid 28-35kg, in and 30-50 minute, measuring the pH value is 6.5～8, gets final product discharging.
2, the described multistep slurry process of claim 1 is characterized in that, the loose density of purified cotton is 〉=120g/l described in the step (3).
3, the described multistep slurry process of claim 1 is characterized in that, comprises the steps:
(1) in three reactors, injects 2 tons of ternary double solventss respectively;
(2) No. 1 reactor is warming up to 22 ℃, vacuumizes, open clean-out cover, drop into sheet alkali 475kg, be warming up to 72 ℃ earlier, at 55 ℃ of constant temperature, continuously stirring 100 minutes;
(3) No. 2 reactors are warming up to 72 ℃, are cooled to 18 ℃ then, vacuumize, open clean-out cover, drop into purified cotton 550kg, at 25 ℃ of following constant temperature, continuously stirring 100 minutes;
(4) drop into Mono Chloro Acetic Acid 450kg to No. 3 reactors, at 35 ℃ of constant temperature, continuously stirring 200 minutes;
(5) No. 1 reactor is vacuumized, after the purified cotton powder in No. 2 reactors stuck with paste through being forced into 4mpa inject in No. 1 reactor, the back adds nitrogen to 2mpa, 3 times repeatedly, at 35 ℃ of constant temperature, continuously stirring 100 minutes;
(6) No. 1 reactor is vacuumized, after the Mono Chloro Acetic Acid in No. 3 reactors be forced into 4mpa inject in No. 1 reactor, the back adds nitrogen to 2mpa, 4 times repeatedly, at 36 ℃ of constant temperature, continuously stirring 125 minutes;
(7) No. 1 reactor is vacuumized, the back adds acetic acid 30kg, in and 40 minutes, measuring the pH value is 7, gets final product discharging.
4, the described multistep slurry process of claim 1 is characterized in that, the ternary double solvents is made up of following component described in the step (1): A, Virahol 78%, B, ethanol 14%, C, soft water 8%.
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Non-Patent Citations (4)
| Title |
|---|
| 聚阴离子纤维素的工艺研究. 吴仁涛.天津化工，第2000年第5期. 2000 |
| 聚阴离子纤维素的工艺研究. 吴仁涛.天津化工，第5期. 2000 * |
| 高性能聚阴离子纤维素处理剂的研制. 朱刚卉.上海化工，第30卷第6期. 2005 |
| 高性能聚阴离子纤维素处理剂的研制. 朱刚卉.上海化工，第30卷第6期. 2005 * |
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