CN101187080A - Use of bamboo pulp synthesized acetyl cellulose in producing acetate silk for textile - Google Patents
Use of bamboo pulp synthesized acetyl cellulose in producing acetate silk for textile Download PDFInfo
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- CN101187080A CN101187080A CNA2006100976419A CN200610097641A CN101187080A CN 101187080 A CN101187080 A CN 101187080A CN A2006100976419 A CNA2006100976419 A CN A2006100976419A CN 200610097641 A CN200610097641 A CN 200610097641A CN 101187080 A CN101187080 A CN 101187080A
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Abstract
The invention discloses the application of a cellulose acetate which is synthesized by bamboo pulp for producing acetate silk for textile. The cellulose acetate which is synthesized by the bamboo pulp is used to produce the cellulose acetate filaments for textile not only is capable of effectively releasing the shortage situation of demands for wood pulp in china, but also is capable of driving the development of bamboo resources processing industry in china. The production of the raw material of the cellulose acetate filaments for textile is wide, and the cost is low.
Description
Technical field:
The present invention relates to a kind of weaving acetate fibre.
Background technology;
Because acetate fibre filament exactly likes town silk most in chemical fibre, gloss is soft, feel light, smooth, the good springiness that softens, drapability is good, is good textile material, therefore receives global concern, development is very fast abroad, but the production of weaving acetate fibre filament still belongs to blank.
Acetic acid synthesized in the world cellulosic be raw material usually with the wood pulps.Because wood pulp is a kind of very special commodity, main cause is raw material restriction, technical limitations, output investment ratio is bigger, the risk height adds the restriction of forest resourceies, problem of environmental pollution etc., present stage is in the seller's market substantially, the manufacturer is few, and the new entrant has still less had how tame production firm to close acetify level wood pulps factory in the world.China's acetic acid synthesized cellulosic raw material wood pulp at present mainly also relies on import, and the situation that wood pulps is in short supply has become the bottleneck of acetate fiber industrial development.
Summary of the invention:
The object of the present invention is to provide a kind of is that the synthetic cellulose acetate of raw material is being produced weaving application in the fine long filament with vinegar with the bamboo pulp.
Technical solution of the present invention is:
The synthetic cellulose acetate of a kind of bamboo pulp is being produced weaving application in the fine long filament with vinegar.
The degree of acetylation that with the bamboo pulp is the synthetic cellulose acetate of main raw material is 52～57%, and average degree of polymerization is 200～500.
Adopting bamboo pulp is the manufacture method of the cellulose acetate made of raw material: comprise the following steps: successively
(1) bamboo pulp is pulverized: with the R-10 value is 50%～99%, and viscosity is that the tabular or cotton-shaped bamboo pulp finished product of 3dl/g～9dl/g is ground into velvet-like by grinder;
(2) activation: acetic acid or aqueous acetic acid are sprayed on the bamboo pulp after the pulverizing, perhaps bamboo pulp are immersed in acetic acid or the aqueous acetic acid, carry out activation processing;
(3) acetylation: acetylation is that solvent, aceticanhydride are that acetylizing agent, sulfuric acid are catalyst with acetic acid, with bamboo 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 bamboo 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 acetylation, and make it precipitating;
(6) washing: adopt demineralized 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 dried, with the moisture Control of cellulose acetate product 1～5%, product.
The consumption of acetic acid is 10%～100% of a bamboo pulp weight during activation processing, and the temperature of activation is 20～40 ℃, soak time 30～300 minutes.
The initial temperature of acetylization reaction is from-10 ℃～20 ℃, and temperature rise rate is controlled at 0.5 ℃/min～3.0 ℃/min, and the time of acetylization reaction was controlled at 20～80 minutes.In view of the reactivity worth of bamboo pulp is better than the reactivity worth of wood pulps, temperature rise rate preferably is controlled at 0.6～0.8 ℃/min, and the acetylization reaction time preferably is controlled at 20～40min.
During hydrolysis, hydrolytic reagent divides 2～4 addings, and the temperature of hydrolytic process is controlled at 70～200 ℃, and when washing was handled, washing temperature was controlled at 40～90 ℃, and the washing time is 20～120 minutes.
R-10 represents to be used for to make the content of the bamboo pulp long chain cellulose of cellulose acetate, and is relevant with alpha-cellulose content.R-10 can measure according to the method among the ASTM D 1696.Testing scheme is as follows: at first pipette the 10%NaOH solution of 100mL, place 20 ℃ thermostat constant temperature 1 hour; The about 1.5g of the bamboo pulp of weighing bone dry is accurate to 0.0001g; The bamboo pulp of accurate weighing is joined in the 10%NaOH solution of 100mL, fully vibrated 1 minute rapidly, placed thermostat 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 sulfuric acid solution 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 sulfuric acid solution is made into standard liquid in sample filtrate and blank filtrate; Place on the hot plate heating after 5-10 minute respectively in sample solution, blank solution, standard liquid, treat its cooling; In 30 minutes, respectively add the 75mL deionized water, and respectively add 3 adjacent coffee sieve quinoline iron ammonium sulfate 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 bamboo pulp by following formula.
In the formula, V0 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 bamboo pulp, g.
The present invention is by being that the synthetic cellulose acetate of raw material is used to produce weaving acetate fibre filament and can not only effectively alleviates domestic nervous situation to the wood pulps demand with bamboo pulp, and can drive the development of domestic bamboo resource secondary industry.Make production weaving acetate fibre filament raw material extensive, cost is low.What the present invention was used is the acetate fibre filament of raw material with the bamboo pulp, its fracture strength is 1.0～1.8g/d (ASTM D2256), 200～240 ℃ of softening points, proportion 1.3～1.4,250～270 ℃ of fusing points are that the long filament of taking of raw material is compared with wood pulps, cotton linter, antibacterial ability obviously strengthens, effectively remove peculiar smell, anti-moth performance obviously improves, and have that dyeing is bright-coloured, antistatic, good hand touch, easy characteristic such as cutting and weaving processing.
The invention will be further described below in conjunction with embodiment.
The specific embodiment:
Embodiment 1:
Adopting bamboo pulp earlier is that raw material is made cellulose acetate, comprises the following steps: successively
(1) bamboo pulp is pulverized: with the R-10 value is 50%～99%, and viscosity is that the tabular or cotton-shaped bamboo pulp finished product of 3dl/g～9dl/g is ground into velvet-like by grinder;
(2) activation: acetic acid or aqueous acetic acid are sprayed on the bamboo pulp after the pulverizing, perhaps bamboo pulp are immersed in acetic acid or the aqueous acetic acid, carry out activation processing;
(3) acetylation: acetylation is that solvent, aceticanhydride are that acetylizing agent, sulfuric acid are catalyst with acetic acid, with bamboo 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 bamboo 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 acetylation, and make it precipitating;
(6) washing: adopt demineralized 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 dried, with the moisture Control of cellulose acetate product 1～5%, product.
The consumption of acetic acid is 10%～100% of a bamboo pulp weight during above-mentioned activation processing, and the temperature of activation is 20～40 ℃, soak time 30～300 minutes.The initial temperature of acetylization reaction is from-10 ℃～20 ℃, and temperature rise rate is controlled at 0.5 ℃/min～3.0 ℃/min, and the time of acetylization reaction was controlled at 20～80 minutes.In view of the reactivity worth of bamboo pulp is better than the reactivity worth of wood pulps, temperature rise rate preferably is controlled at 0.6～0.8 ℃/min, and the acetylization reaction time preferably is controlled at 20～40min.During hydrolysis, hydrolytic reagent divides 2～4 addings, and the temperature of hydrolytic process is controlled at 70～200 ℃, and when washing was handled, washing temperature was controlled at 40～90 ℃, and the washing time is 20～120 minutes.
Adopting the synthetic cellulose acetate of above-mentioned bamboo pulp is raw material, and adopting the degree of acetylation of raw material is 53.4%, and average degree of polymerization is 250.Dissolving, spinning, the drying and other steps of producing long filament by routine are prepared into weaving acetate fibre filament.The weaving acetate fibre filament that makes has following characteristic: fracture strength is 1.2g/d (ASTM D2256), 212 ℃ of softening points, proportion 1.3,251 ℃ of fusing points.
Embodiment 2:
The synthetic cellulose acetate of bamboo pulp that adopts embodiment 1 same procedure to obtain is a raw material, and adopting the degree of acetylation of raw material is 56.1%, and average degree of polymerization is 450.Dissolving, spinning, the drying and other steps of producing the cellulose acetate long filament by routine are prepared into weaving acetate fibre filament.The weaving acetate fibre filament that makes has following characteristic: fracture strength is 1.7g/d (ASTM D2256), 224 ℃ of softening points, proportion 1.4,253 ℃ of fusing points.
Claims (2)
1. the synthetic cellulose acetate of bamboo pulp is being produced weaving application in the fine long filament with vinegar.
2. the synthetic cellulose acetate of bamboo pulp according to claim 1 is being produced weaving application in the fine long filament with vinegar, and it is characterized in that: the degree of acetylation that with the bamboo pulp is the synthetic cellulose acetate of main raw material is 52～57%, and average degree of polymerization is 200～500.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2006100976419A CN101187080A (en) | 2006-11-15 | 2006-11-15 | Use of bamboo pulp synthesized acetyl cellulose in producing acetate silk for textile |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2006100976419A CN101187080A (en) | 2006-11-15 | 2006-11-15 | Use of bamboo pulp synthesized acetyl cellulose in producing acetate silk for textile |
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| CN101187080A true CN101187080A (en) | 2008-05-28 |
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| Application Number | Title | Priority Date | Filing Date |
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| CNA2006100976419A Pending CN101187080A (en) | 2006-11-15 | 2006-11-15 | Use of bamboo pulp synthesized acetyl cellulose in producing acetate silk for textile |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2012021152A (en) * | 2010-06-17 | 2012-02-02 | ▲楊▼占平 | Production method of diacetylcellulose using bamboo fiber as raw material |
| CN106146673A (en) * | 2016-07-14 | 2016-11-23 | 北方民族大学 | By waste paper cellulose acetate method |
| CN107474146A (en) * | 2016-06-08 | 2017-12-15 | 四川普什醋酸纤维素有限责任公司 | A kind of cellulose diacetate and preparation method thereof |
-
2006
- 2006-11-15 CN CNA2006100976419A patent/CN101187080A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2012021152A (en) * | 2010-06-17 | 2012-02-02 | ▲楊▼占平 | Production method of diacetylcellulose using bamboo fiber as raw material |
| CN107474146A (en) * | 2016-06-08 | 2017-12-15 | 四川普什醋酸纤维素有限责任公司 | A kind of cellulose diacetate and preparation method thereof |
| CN107474146B (en) * | 2016-06-08 | 2019-12-13 | 四川普什醋酸纤维素有限责任公司 | Cellulose diacetate and preparation method thereof |
| CN106146673A (en) * | 2016-07-14 | 2016-11-23 | 北方民族大学 | By waste paper cellulose acetate method |
| CN106146673B (en) * | 2016-07-14 | 2018-11-09 | 北方民族大学 | By waste paper cellulose acetate method |
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Open date: 20080528 |