CN1084816C - Producing process capable of lowering decline of cellulose mucus colour and lustre, and polymerization degree - Google Patents

Producing process capable of lowering decline of cellulose mucus colour and lustre, and polymerization degree Download PDF

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CN1084816C
CN1084816C CN98101642A CN98101642A CN1084816C CN 1084816 C CN1084816 C CN 1084816C CN 98101642 A CN98101642 A CN 98101642A CN 98101642 A CN98101642 A CN 98101642A CN 1084816 C CN1084816 C CN 1084816C
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additive
mucus
cellulose
decline
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CN1195050A (en
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郑孟松
蔡照雄
黄坤山
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JULONG FIBRE CO Ltd
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JULONG FIBRE CO Ltd
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Abstract

The present invention relates to a method for reducing the luster and the polymerization degree decay of cellulose mucus by using an additive. An additive for resisting the polymerization degree decay of 1, 3-phenylene-bis, 2-oxazoline (BOX) is added to mucus, and the luster and the polymerization degree decay of the dissolved mucus are effectively reduced so as to enhance the physical performance of fibrous products and reduce the cost.

Description

Reduce the method for making of cellulose mucus color and luster and degree of polymerization decline
The present invention is a kind of color and luster of cellulose mucus and manufacture method of degree of polymerization decline of reducing, and refers to a kind of with the manufacture method of cellulose dissolution in the solvent of blast blending especially.Belong to the chemical fibre technical field.
General traditional needed flow process of rayon spinning is quite numerous and diverse, spinning speed is slow, consuming time many, and emission of substance such as carbon disulfide, sulfur dioxide, environmental pollution caused quite easily, therefore rayon mucus adopts the mode of production of wet type spinning to reduce gradually, at the shortcoming of above-mentioned traditional rayon spinning, so-called cellulose solvent spin processes is created in exploitation in recent years, to reduce the pollution to environment, but these solvent methods of commonly using are using in the enforcement, still have following point:
1. utilize and commonly use solvent method and dissolve resulting mucus, its viscosity is up to the 8000-12000 dregs of rice (poise), its difficulty in spinning, in order to make it be easy to spinning, then need to adopt the process conditions of higher temperature and long period, with reduction mucus viscosity, however long process conditions of temperature height and time, make the degree of polymerization (DP) of cellulose fail significantly, cause cellulose intensity to reduce.
2. commonly use solvent method under the processing procedure of higher temperature and long period,,, cause the recovery process of solvent must pass through the operation of multiple tracks purifying causing the color and luster of cellulose mucus to deepen easily if do not mix or mix bad anti-degree of polymerization decline additive.
3. commonly use solvent method under the processing procedure of higher temperature and long period, if do not mix or mix bad anti-degree of polymerization decline additive, make the easy cracking of solvent, its rate of recovery is only about 94%, causes the increase of manufacturing cost.
4. the additive of commonly using solvent method be generally gallic acid (n-proply gallate, P.G) and calgon (sodium hexametaphosphate, SHMP), but both costs are too high and effect is little.
In order to overcome above-mentioned deficiency, the objective of the invention is: provide a kind of and can reduce the cellulose mucus color and luster and solve the manufacture method of degree of polymerization decline, it mainly is a blast blending oxazolyl phenyl (1 in mixed solvent, 3-pheny lene-bis 2-oxazoline), use the color and luster of reduction cellulose mucus and the decline of the degree of polymerization, reach the purpose of enhanced products rerum natura and raising fiber quality.
The method for making of the present invention's a kind of reduction cellulose mucus color and luster and degree of polymerization decline, with wood pulp fibre, organic solvent and anti-painted/mixture of anti-degree of polymerization decline additive is dissolved into cellulose mucus through heating, reduce pressure, dewatering; Wherein employed anti-painted/anti-degree of polymerization decline additive is oxazolyl phenyl (1,3-pheny lene-bis 2-oxazoline), the amount of this additive is 500~2500ppm of cellulose amount.
Wherein, this mixture is under 80~100 ℃ of decompression states that add thermal agitation and 50~100mmHg, and moisture content is got rid of to 8~11% promptly becomes cellulose mucus.
Wherein, this additive is when 13.3% cellulose mucus concentration, and its spectrophotometer 470nm color and luster transmitance index is 10.2, and degree of polymerization fading rate is 11.6%.Wherein, the chemical constitution of this additive oxazolyl phenyl (1,3-pheny lene-bis 2-oxazoline) is as follows:
Figure C9810164200041
Advantage of the present invention is; Can reduce the cellulose mucus color and luster effectively and reduce degree of polymerization decline, reinforcing fiber product rerum natura improves fiber quality, reduces manufacturing cost.
Now lifting preferable manufacture process and test examples is described in detail as follows:
The method for making of the present invention's a kind of reduction cellulose mucus color and luster and degree of polymerization decline, wherein, the cellulose-based alpha-cellulose that the present invention adopts, content all is suitable at the long and short fiber more than 90%, and the solvent that adopts is to be mixed into mixed solvent by oxidation methyl woods (N-Methyl Morpholine Oxide) and N-Methylol Caprolactom (N-Methylol Caprolactom) with about 7: 3 part by weight, and is as follows in regular turn as for the manufacturing process that the present invention is concrete:
A. mix anti-degree of polymerization decline additive oxazolyl phenyl, with the color and luster of reduction cellulose mucus and the decline of the degree of polymerization; The chemical constitution of this oxazolyl phenyl is as follows:
Figure C9810164200042
B. utilize kneader to be size mixing equipment, 8% weight fibres element, 46% weight mixed solvent, 46% weight water and additive are mediated under 50~60 ℃ low temperature together;
C. utilize the moisture content of vacuum film evaporating surplus, under 80~100 ℃ of heating and the decompression state of 50~100mmHg, get rid of moisture content to 9~11% in 5 minutes, cellulose dissolution is become mucus;
D. above-mentioned mucus just can obtain fiber or finished film through spinning regeneration, washing and drying process;
E. this solvent can fully recycle, and reduces decline and simplifies refining reason because mix the additive of oxazolyl phenyl, and the coefficient of losses of solvent is quite low, and the rate of recovery can reach more than 99.5%.
So, it is additive that the present invention adopts oxazolyl phenyl, has following characteristic and advantage:
1. mix the anti-degree of polymerization decline additive oxazolyl phenyl (1 of 500~2500ppm in the solvent, 3-pheny lene-bis 2-oxazoline) (ppm that is mixed in this solvent is to be benchmark with the cellulose) reconciles into slurries with wood pulp, see also shown in the table one, this additive has decline of the wood pulp cellulose degree of polymerization and the painted effect of solvolysis of preventing in the course of dissolution.
2. the present invention produces less painted because of mixing the oxazolyl phenyl additive, as shown in Table 2, it chromogenic indicator is that 470nm spectrophotometer transmitance index is reduced to 10.2 (below 15.0) by 51.1 of use gallic acid, can simplify the refining program of solvent recovery, improves solvent recovering rate.
3. the present invention produces less degree of polymerization decline because of mixing the oxazolyl phenyl additive, and shown in table one and table two, its fading rate drops to below 15%.
4. the present invention uses the oxazolyl phenyl as additive, sees also shown in the table three, and gallic acid that its unit price is commonly used and calgon are cheap a lot, help reducing solvent cost.
More than especially as shown in Table 4 with every characteristic tabulation of the present invention and the solvent method of commonly using, to show innovation effect of the present invention.
Table one:
Oxazolyl phenyl adding proportion (ppm) Transmitance index (470nm) Degree of polymerization fading rate (%)
500 20.1 26.2
1000 15.2 20.5
1500 13.8 14.7
2000 10.2 11.6
2500 9.8 11.3
Table two:
Additive types Cellulosic degree of polymerization Cellulose concentration Additive adding proportion (ppm) Transmitance index (470nm) Degree of polymerization fading rate (%)
Calgon 950 13.3% 2000 46.8 26.1
Gallic acid 950 13.3% 2000 51.1 26.7
Oxazolyl phenyl 950 13.3% 2000 10.2 11.6
Table three: (unit: dollar/kilogram)
Additive types Unit price Additive adding proportion (ppm) The additive cost
Calgon 30.30 2000 0.27
Gallic acid 848.48 2000 7.50
Oxazolyl phenyl 29.09 2000 0.26
Table four:
The mucus rerum natura The present invention Commonly use method
Oxazolyl phenyl Gallic acid Calgon
Content of cellulose (%) 11.0 11.9 10.1
Solvent (%) 81.6 73.2 79.1
Water content (%) 7.4 14.9 10.8
Mucus viscosity (poise/100C) 10120 13000 11780
Degree of polymerization fading rate (%) 11.6 26.7 26.1
Transmitance index (470nm) 10.2 51.1 46.8
Solvent recovering rate (%) 99.5 95.0 96.0

Claims (4)

1, the method for making of a kind of reduction cellulose mucus color and luster and degree of polymerization decline is characterized in that: with wood pulp fibre, organic solvent and anti-painted/mixture of anti-degree of polymerization decline additive is dissolved into cellulose mucus through heating, reduce pressure, dewatering; Wherein employed anti-painted/anti-degree of polymerization decline additive is oxazolyl phenyl (1,3-pheny lene-bis 2-oxazoline), the amount of this additive is 500~2500ppm of cellulose amount.
2. the method for making of a kind of reduction cellulose mucus color and luster according to claim 1 and degree of polymerization decline, it is characterized in that: wherein, this mixture is under 80~100 ℃ of decompression states that add thermal agitation and 50~100mmHg, and moisture content is got rid of to 8~11% promptly becomes cellulose mucus.
3. the method for making of a kind of reduction cellulose mucus color and luster according to claim 1 and degree of polymerization decline, it is characterized in that: wherein, this additive is when 13.3% cellulose mucus concentration, and its spectrophotometer 470nm color and luster transmitance index is 10.2, and degree of polymerization fading rate is 11.6%.
4. the method for making of a kind of reduction cellulose mucus color and luster according to claim 1 and degree of polymerization decline is characterized in that: wherein, the chemical constitution of this additive oxazolyl phenyl (1,3-pheny lene-bis2-oxazoline) is as follows:
Figure C9810164200021
CN98101642A 1998-04-24 1998-04-24 Producing process capable of lowering decline of cellulose mucus colour and lustre, and polymerization degree Expired - Fee Related CN1084816C (en)

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CN102127841B (en) * 2010-01-13 2014-07-16 聚隆纤维股份有限公司 Production method of cellulose non-woven fabric with functions of mildew proofing, antibiosis and deodorization through wet-type meltbrown
CN102127840B (en) * 2010-01-13 2014-07-16 聚隆纤维股份有限公司 Method for preparing natural cellulose non-woven fabric in wet spunbond mode
TWI509008B (en) * 2012-12-14 2015-11-21 A method for preparing artificial water moss with natural cellulose fibers
CN103215753B (en) * 2013-03-26 2016-01-13 聚隆纤维股份有限公司 There is the method for making of deodorization functions bamboo pulp fiber element Nonwovens

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