CN101544698A - Cellulose acetate prepared by taking cotton linter pulp as raw material and preparation method and application thereof - Google Patents
Cellulose acetate prepared by taking cotton linter pulp as raw material and preparation method and application thereof Download PDFInfo
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- CN101544698A CN101544698A CN200910030549A CN200910030549A CN101544698A CN 101544698 A CN101544698 A CN 101544698A CN 200910030549 A CN200910030549 A CN 200910030549A CN 200910030549 A CN200910030549 A CN 200910030549A CN 101544698 A CN101544698 A CN 101544698A
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Abstract
The invention discloses cellulose acetate prepared by taking cotton linter pulp as the raw material and a preparation method and an application thereof. The cellulose acetate is prepared by pulverizing, activating, acetylizing, hydrolyzing, precipitating, rinsing and drying the cotton linter pulp which is used as the raw material. The cellulose acetate is used for manufacturing textile cellulose acetate filaments, membranes, semipermeable membranes, photosensitive films and other materials. The cellulose acetate is prepared by taking cotton linter pulp as the raw material which is easy to obtain, and the preparation method of the cellulose acetate is easy to operate and ensures good product quality.
Description
Technical field:
The present invention relates to adopt cotton linter dissolving pulp is cellulose acetate and the manufacture method and the purposes of feedstock production.
Background technology:
At present, acetic acid synthesized cellulosic pulp raw material is generally from wood pulps.Since the restriction of forest resourceies, the tooling cost height of wood pulps, and problem of environmental pollution is serious, has had how tame production firm to close acetify level wood pulps factory in the world.Because the shortage of wood pulps supply, China's acetic acid synthesized cellulosic raw material at present mainly also relies on import, has limited domestic cellulose acetate industrial expansion to a great extent.
China is maximum in the world cotton linter dissolving pulp producing country, aboundresources, and the output of the domestic dissolving grade cotton pulp dregs of rice reaches 800,000 tons, and major part only is used for the cheap inferior grade products such as viscose fiber of production prices.The cotton pulp dregs of rice have characteristics such as chemical cellulose content height, polymerization degree homogeneous, impurity content are low, have the feasibility of preparation cellulose acetate.
Therefore adopt cotton linter dissolving pulp can not only alleviate domestic nervous situation, can promote the deep processing and the utilization thereof of domestic agricultural-food simultaneously the wood pulps demand for the feedstock production cellulose acetate.But adopt cotton linter dissolving pulp to prepare cellulose acetate suitable difficulty is arranged technically, mainly show cotton linter dissolving pulp degree of crystallinity height, the difficult control of acetylation, and production efficiency is low.
Summary of the invention:
The object of the present invention is to provide a kind of raw material to be easy to get, good product quality be cellulose acetate and manufacture method and the purposes that raw material is made with the cotton linter dissolving pulp.
Technical solution of the present invention is:
A kind of is the cellulose acetate that raw material is made with the cotton linter dissolving pulp, it is characterized in that: be to be raw material with the cotton linter dissolving pulp, and the product that makes through pulverizing, activation, acetylize, hydrolysis, precipitating, washing, drying.
The R-10 value of raw material cotton linter dissolving pulp is 80%～99.5%, and viscosity is 4dl/g～10dl/g.
A kind of is the manufacture method of the cellulose acetate made of raw material with the cotton linter dissolving pulp, it is characterized in that: comprise the following steps: successively
(1) cotton linter dissolving pulp is pulverized: with the R-10 value is 80%～99.5%, and viscosity is that the tabular cotton linter dissolving pulp finished product of 4dl/g～10dl/g is ground into velvet-like by shredder;
(2) activation: acetic acid or aqueous acetic acid are sprayed on the cotton linter dissolving pulp after the pulverizing, perhaps cotton linter dissolving pulp are immersed in acetic acid or the aqueous acetic acid, carry out activation treatment; The consumption of acetic acid is 10%～100% of a cotton linter dissolving pulp weight during activation treatment, and the activatory temperature is 20～40 ℃, soak time 30～300 minutes;
(3) acetylize: acetylation is that solvent, aceticanhydride are that acetylizing agent, sulfuric acid are catalyzer with acetic acid, with cotton linter dissolving pulp weight is benchmark, the aceticanhydride of the sulfuric acid of the acetic acid of 20～800% weight, 3～25% weight, 50～500% weight and cotton linter dissolving pulp is added in the reactor carry out acetylization reaction;
(4) hydrolysis: to adopt mass concentration be 10～30% the magnesium acetate aqueous solution as the hydrolytic reagent reaction that is hydrolyzed;
(5) precipitating: the slurry dilution after the dilute acetic acid solution of employing 3～10% concentration is finished acetylize, and make it precipitating;
(6) washing: adopt softening water that the cellulose acetate that separates out is washed processing;
(7) drying: under 90 ℃～120 ℃ conditions cellulose acetate after the washing is being carried out drying treatment, with the moisture controlled of cellulose acetate product 1～5%, product.
The initial temperature of acetylization reaction is from-20 ℃～20 ℃, and temperature rise rate is controlled at 0.5 ℃/min～1.2 ℃/min, and the time of acetylization reaction was controlled at 80～100 minutes.
During hydrolysis, hydrolytic reagent divides 2～4 addings, and the temperature of hydrolytic process is controlled at 70～200 ℃.
When washing was handled, washing temperature was controlled at 40～90 ℃, and the washing time is 20～120 minutes.
A kind of cellulose acetate that with the cotton linter dissolving pulp is raw material is made is preparing the application of cigarette with cellulose acetate, weaving acetate fibre filament, polarizer protective membrane, colour filter, the film that is used for photochromics, semipermeable partition or sensitive film.
By being carried out acetylize, cotton linter dissolving pulp produces cellulose acetate of the present invention.Kind for cotton linter dissolving pulp does not have special requirement, can use the cotton linter dissolving pulp in various sources, comprises the cotton linter dissolving pulp that has been used for papermaking and viscose fibre industry at present.According to the present invention, acetic acid synthesized cellulosic raw material cotton linter dissolving pulp possesses following index:
(1)R-10∶80％～99.5％
(2) viscosity: 4dl/g～10dl/g
R-10 represents to be used for to make the content of the numb oar dregs of rice long chain cellulose of cellulose acetate, and is relevant with α-content of cellulose.R-10 can measure according to the method among the ASTM D1696.Testing scheme is as follows: at first pipette the 10%NaOH solution of 100mL, place 20 ℃ thermostatic bath constant temperature 1 hour; The about 1.5g of the cotton linter dissolving pulp of weighing complete drying is accurate to 0.0001g; The cotton linter dissolving pulp of accurate weighing is joined in the 10%NaOH solution of 100mL, fully vibrated 1 minute rapidly, placed thermostatic bath then 1 hour; The NaOH solution that pipettes 100mL filters through sand core funnel as blank solution, and sample solution is also filtered through sand core funnel; The sample filtrate and the blank filtrate branch that pipette 15mL are clipped in two Erlenmeyer flasks, the sulphuric acid soln that adds the 0.0833M potassium bichromate solution of 10mL and 30mL respectively gets that a clean 250mL Erlenmeyer flask adds the 10mL potassium bichromate solution and the 30mL sulphuric acid soln is made into standardized solution in sample filtrate and blank filtrate; Place on the hot plate heating after 5-10 minute respectively in sample solution, blank solution, standardized solution, treat its cooling; In 30 minutes, respectively add the 75mL deionized water, and respectively add 3 adjacent coffee sieve quinoline ferrous ammonium sulphate indicator, and carry out titration respectively with the 0.1M ammonium ferric sulfate solution, read titration volume number, be accurate to 0.01mL, and calculate the R-10 value of cotton linter dissolving pulp by following formula.
In the formula, VO represents blank titration volume, mL; V1 represents sample titration volume, mL;
V2 represents the volume number of the sulfurous acid iron ammonium that timing signal consumes, mL; N represents the equivalent concentration of potassium bichromate; W represents the dry weight of cotton linter dissolving pulp, g.
The viscosity index of cotton linter dissolving pulp has reflected its polymerization degree size, can measure according to following method.Get the 120mL vial, 30mL water is stand-by to wherein adding.The oven dry fiber crops oar dregs of rice of weighing 150mg are accurate to 0.1mg.It is added in the vial, vibrated rapidly 1 minute, place again on the vibrator and vibrated 15 minutes.The mother glass bottle is placed nitrogen chamber, connected nitrogen 3-5 minute.Outward winding in the nitrogen chamber spiral cover of mother glass bottle is to 1M copper second two ammonium solutions that wherein add 30mL.Be statically placed in the nitrogen chamber after 1-2 minute, screw lid.After the quick oscillation 30 seconds, place on the vibrator, vibrated 10 minutes.(CANNON, 150mL 133A), swing to and draw sample solution to the second scale marks to get special-purpose viscometer.The viscometer forward is vertically put into 25 ± 0.05 ℃ thermostatic bath, left standstill 10 minutes.Sample solution is drawn to first scale marks, it is freely fallen.Drop to the time t (second) of second scale marks from first scale marks with stopwatch statistics liquid level.According to following formula calculated characteristics viscosity.
Degree of acetylation is represented the binding capacity of acetate in the cellulose acetate product, and is expressed as the weight percent of every Mierocrystalline cellulose unit weight bonded acetate.Degree of acetylation can be measured according to the method that is used to measure degree of acetylation among the ASTM D871-96 (testing method of cellulose acetate etc.).Measurement scheme is as follows: at first accurate weighing 1.9 gram exsiccant cellulose acetates, (4:1 in mixture v/v), adds the aqueous sodium hydroxide solution of 30ml 1N, and saponification 2 hours under 25 ℃ of conditions to be dissolved in 150ml acetone-dimethyl sulfoxide (DMSO).Add 2～3 phenolphthalein indicators, and with the sodium hydroxide of the sulfuric acid overtitration of 1N.Carry out blank test with above-mentioned same method, and calculate degree of acetylation by following equation:
Degree of acetylation (%)=(6.5 * (B-A) * F)/W
In the formula, A represents to add to 1N vitriolic consumption (ml) in the sample, and B represents to add to 1N vitriolic consumption (ml) in the check sample, and F represents 1N vitriolic concentration factor, and W is the weight (g) of sample.
With the viscometric degree of polymerization is unit, and the polymerization degree of cellulose acetate is from 200～600, preferably from 250～400.Mean polymerisation degree can be measured (KazuoUda﹠amp by people's such as Uda limiting viscosity method; Hideo Saito:Journal of the Society of Fiber Science andTechnology, Japan, Vol.18, No.1 105-120,1962).In the method, can come selective solvent according to the degree of acetylation of cellulose acetate.For example, in the occasion of cellulosetri-acetate, testing program is as follows:
Cellulosetri-acetate is dissolved in the mixture of methylene dichloride-methyl alcohol (9:1 weight ratio) of finite concentration c (2.00g/l), then this solution is injected Ostward viscometer and measure this solution mobile time t between the viscometer scale at 25 ℃.On the other hand, measure blank flowing time (second), and calculate viscometric degree of polymerization by means of following formula with above-mentioned solvent mixture:
η
rel＝t/t
0
[η]＝(lnη
rel)/c
Dp＝[η]/(6×10
-4)
T represents the flowing time (second) of solution, t in the formula
0The flowing time (second) of expression solvent, c represents the strength of solution (g/l) of cellulosetri-acetate, η
RelThe expression relative viscosity, [η] representation feature viscosity, Dp is a mean polymerisation degree.
The cellulose acetate of the present invention's preparation is raw material with the cotton linter dissolving pulp; raw material is easy to get; manufacture method is simple, easy to operate; good product quality is applicable to and produces cigarette with materials such as cellulose acetate, weaving acetate fibre filament, film (polarizer protective membrane, colour filter, be used for the film of photochromics), semipermeable partition, sensitive films.
The invention will be further described below in conjunction with embodiment:
Embodiment:
Embodiment 1:
With the cotton linter dissolving pulp that R-10 is 85.6%, viscosity is 5.7dl/g is raw material, through following prepared cellulose acetate:
(1) cotton linter dissolving pulp is pulverized: tabular cotton linter dissolving pulp finished product is ground into velvet-like outward appearance by shredder.
(2) activation: acetic acid is sprayed on the cotton linter dissolving pulp after the pulverizing.The consumption of acetic acid is 80% of a cotton linter dissolving pulp weight, and the activatory temperature is 25 ℃, soak time 100 minutes.
(3) acetylize: with cotton linter dissolving pulp weight is benchmark; acetic acid with 300%, 18% sulfuric acid, 200% aceticanhydride and cotton linter dissolving pulp add in the acetify reactor; the initial temperature of reaction is from-10 ℃, and temperature rise rate is controlled to be 1 ℃/min, and the time of acetylization reaction is 80 minutes.
(4) hydrolysis: adopt mass concentration be 20% the magnesium acetate aqueous solution as hydrolytic reagent, begin to add at twice in back 1 hour, 1.5 hours in hydrolysis.The temperature of hydrolytic process is controlled at 85 ℃.After 1.5 hours, end hydrolysis reaction.
(5) precipitating: the slurry dilution after adopting the dilute acid soln of 10% concentration that acetylize is finished, and make it precipitating.
(6) washing: adopt softening water that the cellulose acetate that separates out is washed, washing temperature is 80 ℃, and the washing time is 100min.
(7) drying: under 105 ℃ of conditions the cellulose acetate after the washing is being carried out warm air drying, the moisture controlled of final cellulose acetate product is 3%.
The degree of acetylation that present embodiment finally prepares cellulose acetate is 58.9%, and mean polymerisation degree is 340.Can be applicable to the preparation of materials such as film (polarizer protective membrane, colour filter, be used for the film of photochromics), semipermeable partition, sensitive film.
Embodiment 2:
With the cotton linter dissolving pulp that R-10 is 99.1%, viscosity is 8.2dl/g is raw material, through following prepared cellulose acetate:
(1) cotton linter dissolving pulp is pulverized: cotton-shaped cotton linter dissolving pulp finished product is ground into velvet-like outward appearance by shredder.
(2) activation: acetic acid is sprayed on the cotton linter dissolving pulp after the pulverizing.The consumption of acetic acid is 18% of a cotton linter dissolving pulp weight, and the activatory temperature is 30 ℃, soak time 50 minutes.
(3) acetylize: with cotton linter dissolving pulp weight is benchmark; acetic acid with 300%, 8% sulfuric acid, 220% aceticanhydride and cotton linter dissolving pulp add in the acetify reactor; the initial temperature of reaction is since 0 ℃, and temperature rise rate is controlled to be 0.85 ℃/min, and the time of acetylization reaction is 96 minutes.
(4) hydrolysis: adopt mass concentration be 20% the magnesium acetate aqueous solution as hydrolytic reagent, begin back 1 hour, 2.5 hours, 4 little time-divisions in hydrolysis and add for three times.The temperature of hydrolytic process is controlled at 82 ℃.After 4 hours, end hydrolysis reaction.
(5) precipitating: the slurry dilution after adopting the dilute acid soln of 10% concentration that acetylize is finished, and make it precipitating.
(6) washing: adopt softening water that the cellulose acetate that separates out is washed, washing temperature is 80 ℃, and the washing time is 100min.
(7) drying: under 105 ℃ of conditions the cellulose acetate after the washing is being carried out warm air drying, the moisture controlled of final cellulose acetate product is 3%.
The degree of acetylation that present embodiment finally prepares cellulose acetate is 55.6%, and mean polymerisation degree is 410.Can be applicable to the preparation of cigarette with cellulose acetate, weaving acetate fibre filament.
Claims (7)
1, a kind of is the cellulose acetate that raw material is made with the cotton linter dissolving pulp, it is characterized in that: be to be raw material with the cotton linter dissolving pulp, and the product that makes through pulverizing, activation, acetylize, hydrolysis, precipitating, washing, drying.
2, employing cotton linter dissolving pulp according to claim 1 is the cellulose acetate that raw material is made, and it is characterized in that: the R-10 value of raw material cotton linter dissolving pulp is 80%～99.5%, and viscosity is 4dl/g～10dl/g.
3, a kind of is the manufacture method of the cellulose acetate made of raw material with the cotton linter dissolving pulp, it is characterized in that: comprise the following steps: successively
(1) cotton linter dissolving pulp is pulverized: with the R-10 value is 80%～99.5%, and viscosity is that the tabular cotton linter dissolving pulp finished product of 4dl/g～10dl/g is ground into velvet-like by shredder;
(2) activation: acetic acid or aqueous acetic acid are sprayed on the cotton linter dissolving pulp after the pulverizing, perhaps cotton linter dissolving pulp are immersed in acetic acid or the aqueous acetic acid, carry out activation treatment; The consumption of acetic acid is 10%～100% of a cotton linter dissolving pulp weight during activation treatment, and the activatory temperature is 20～40 ℃, soak time 30～300 minutes;
(3) acetylize: acetylation is that solvent, aceticanhydride are that acetylizing agent, sulfuric acid are catalyzer with acetic acid, with cotton linter dissolving pulp weight is benchmark, the aceticanhydride of the sulfuric acid of the acetic acid of 20～800% weight, 3～25% weight, 50～500% weight and cotton linter dissolving pulp is added in the reactor carry out acetylization reaction;
(4) hydrolysis: to adopt mass concentration be 10～30% the magnesium acetate aqueous solution as the hydrolytic reagent reaction that is hydrolyzed;
(5) precipitating: the slurry dilution after the dilute acetic acid solution of employing 3～10% concentration is finished acetylize, and make it precipitating;
(6) washing: adopt softening water that the cellulose acetate that separates out is washed processing;
(7) drying: under 90 ℃～120 ℃ conditions cellulose acetate after the washing is being carried out drying treatment, with the moisture controlled of cellulose acetate product 1～5%, product.
4, according to claim 3 is the manufacture method of the cellulose acetate made of raw material with the cotton linter dissolving pulp; it is characterized in that: the initial temperature of acetylization reaction is from-20 ℃～20 ℃; temperature rise rate is controlled at 0.5 ℃/min～1.2 ℃/min, and the time of acetylization reaction was controlled at 80～100 minutes.
5, according to claim 3 or 4 described be the manufacture method of the cellulose acetate made of raw material with the cotton linter dissolving pulp, it is characterized in that: during hydrolysis, hydrolytic reagent divides 2～4 addings, and the temperature of hydrolytic process is controlled at 70～200 ℃.
6, according to claim 3 or 4 described be the manufacture method of the cellulose acetate made of raw material with the cotton linter dissolving pulp, it is characterized in that: when washing was handled, washing temperature was controlled at 40～90 ℃, and the washing time is 20～120 minutes.
7, a kind of claim 1 is described is that the cellulose acetate that raw material is made is preparing the application of cigarette with cellulose acetate, weaving acetate fibre filament, polarizer protective membrane, colour filter, the film that is used for photochromics, semipermeable partition or sensitive film with the cotton linter dissolving pulp.
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| CN101845100A (en) * | 2010-06-17 | 2010-09-29 | 杨占平 | Method for manufacturing cellulose diacetate by using natural bamboo fiber as raw material |
| CN102120775A (en) * | 2010-12-06 | 2011-07-13 | 江南大学 | Acetylation thermoplastic modification method of rice straw |
| CN102936289A (en) * | 2012-12-10 | 2013-02-20 | 西安北方惠安化学工业有限公司 | Preparation method of optical cellulose triacetate |
| CN105178081A (en) * | 2015-09-17 | 2015-12-23 | 河北吉藁化纤有限责任公司 | Preparation method of acetified cotton pulp and pulp prepared by preparation method |
| CN110078836A (en) * | 2019-04-18 | 2019-08-02 | 中峰化学有限公司 | The preparation method of the cellulose acetate of big plate degree of substitution |
| CN111379184A (en) * | 2018-12-28 | 2020-07-07 | 安徽雪龙纤维科技股份有限公司 | Cotton pulp for producing cellulose acetate butyrate and preparation method thereof |
| CN111621864A (en) * | 2020-04-25 | 2020-09-04 | 武汉裕大华纺织有限公司 | Production process of acetate fiber variety |
| CN114587006A (en) * | 2021-05-25 | 2022-06-07 | 武汉达汇新科技有限公司 | Preparation method for improving tobacco sheets by adopting modified low-polymerization-degree cotton linter pulp |
| CN114736311A (en) * | 2022-05-09 | 2022-07-12 | 国际竹藤中心 | Bamboo-derived cellulose acetate and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101845100A (en) * | 2010-06-17 | 2010-09-29 | 杨占平 | Method for manufacturing cellulose diacetate by using natural bamboo fiber as raw material |
| CN101845100B (en) * | 2010-06-17 | 2012-06-27 | 杨占平 | Method for manufacturing cellulose diacetate by using natural bamboo fiber as raw material |
| CN102120775A (en) * | 2010-12-06 | 2011-07-13 | 江南大学 | Acetylation thermoplastic modification method of rice straw |
| CN102120775B (en) * | 2010-12-06 | 2012-08-29 | 江南大学 | Acetylation thermoplastic modification method of rice straw |
| CN102936289A (en) * | 2012-12-10 | 2013-02-20 | 西安北方惠安化学工业有限公司 | Preparation method of optical cellulose triacetate |
| CN102936289B (en) * | 2012-12-10 | 2014-12-03 | 西安北方惠安化学工业有限公司 | Preparation method of optical cellulose triacetate |
| CN105178081A (en) * | 2015-09-17 | 2015-12-23 | 河北吉藁化纤有限责任公司 | Preparation method of acetified cotton pulp and pulp prepared by preparation method |
| CN105178081B (en) * | 2015-09-17 | 2017-07-18 | 河北吉藁化纤有限责任公司 | A kind of vinegar-grade Cotton Pulp preparation method and its pulp of preparation |
| CN111379184A (en) * | 2018-12-28 | 2020-07-07 | 安徽雪龙纤维科技股份有限公司 | Cotton pulp for producing cellulose acetate butyrate and preparation method thereof |
| CN110078836A (en) * | 2019-04-18 | 2019-08-02 | 中峰化学有限公司 | The preparation method of the cellulose acetate of big plate degree of substitution |
| CN111621864A (en) * | 2020-04-25 | 2020-09-04 | 武汉裕大华纺织有限公司 | Production process of acetate fiber variety |
| CN114587006A (en) * | 2021-05-25 | 2022-06-07 | 武汉达汇新科技有限公司 | Preparation method for improving tobacco sheets by adopting modified low-polymerization-degree cotton linter pulp |
| CN114587006B (en) * | 2021-05-25 | 2024-02-27 | 武汉达汇新科技有限公司 | Preparation method for improving tobacco sheet by adopting modified cotton linter pulp with low polymerization degree |
| CN114736311A (en) * | 2022-05-09 | 2022-07-12 | 国际竹藤中心 | Bamboo-derived cellulose acetate and preparation method thereof |
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