CN1084813C - Method for producing low-viscosity cellulose mucus - Google Patents
Method for producing low-viscosity cellulose mucus Download PDFInfo
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- CN1084813C CN1084813C CN98101641A CN98101641A CN1084813C CN 1084813 C CN1084813 C CN 1084813C CN 98101641 A CN98101641 A CN 98101641A CN 98101641 A CN98101641 A CN 98101641A CN 1084813 C CN1084813 C CN 1084813C
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Abstract
The present invention relates to a preparing method of low-viscosity cellulose mucus. In the method, n-methylol caprolactom is used as a second solvent, and the second solvent is mixed with n-methyl morpholine oxide as a main solvent, so the bulkness of fibers is improved and the solution composition is changed in the process of dissolution so that the cellulose mucus achieves the effect of reducing the viscosity of cellulose mucus; simultaneously, because of the effect, low-temperature dissolution and high-speed spinning can be adopted in the preparing process, the decline of the cellulose polymerization degree can be effectively reduced, the physical property of the fiber products can be reinforced, and the quality of the products can be improved.
Description
The present invention is a kind of method for producing low-viscosity cellulose mucus, refers to that especially a kind of use second solvent in main solvent, reaches the improvement solvent properties, and then makes the method for low-viscosity cellulose mucus, belongs to the chemical fibre technical field.
The processing procedure of traditional fibre cellulose fiber mainly is to adopt viscose process, because the making long flow path of viscose process, and production process can produce carbon disulfide (CS
2), sulfur dioxide (SO
2), cause air pollution and water to pollute, so its output is stagnated.Free of contamination in recent years cellulose solvent spin processes (hereinafter to be referred as " solvent method ") through long-term test, has had produced in small quantities, and solvent method is except pollution-free, advantage such as have still that processing procedure is short, output is big, cost low and product performance is good; Yet the conventional well-known solvents method causes difficulty in spinning because of viscosity high [reaching the 8000-12000 dregs of rice (poise)] at present, must reduce the solution cellulose concentration or improve spinning temperature, low cellulose concentration not only can reduce output, and increase solvent load and cost recovery, the high spinning temperature then causes the fiber degree of polymerization (DP) to decline to a great extent easily, reduce product intensity, these all are the technical problems that solvent method haves much room for improvement.
In addition, dimethyl oxidation sulphur (DMSO, Dimethyl Sulfoxide) often is studied in improving solution viscosity, but because its be not easy to obtain and effect bad, therefore can't formally adopt.
A kind of method for producing low-viscosity cellulose mucus of the present invention, its objective is: a kind of method for producing low-viscosity cellulose mucus that utilizes solvent method to reduce cellulose mucus viscosity is provided, it mainly is with the main solvent oxidation methyl woods and the second solvent N-Methylol Caprolactom, adopt certain ratio to be mixed, the viscosity of mucus after not only can increasing the moistening ability (swelling) of the preceding wood pulp of dissolving and reducing dissolving, and can and then improve cellulosic dissolubility and spinnability.
A kind of method for producing low-viscosity cellulose mucus, the mixture that comprises wood pulp fibre, mixed solvent and stabilization agent forms cellulose mucus through heating, reduce pressure, remove water-soluble; It is characterized in that: this mixed solvent comprises the combined type solvent of main solvent oxidation methyl woods (N-Methyl Morpholine Oxide) and secondary solvent N-Methylol Caprolactom (N-Methylol Caprolactom), just, the mixed proportion of secondary solvent is 7 to 3; This mixed solvent total amount is 5.5～7.5 times of cellulose amount; This mixed solvent, when 12% cellulose mucus concentration, its viscosity is 6,500 dregs of rice (poise).
Wherein, 46% weight mixed solvent, 46% weight water and 8% weight wood pulp cellulose, and with wood pulp cellulose weight be benchmark 5000ppm anti-polymerization decline additive in 60 ℃ mixed, evaporation removes moisture content to 10% weight in the mixed liquor that is obtained and forms this low-viscosity cellulose mucus.Wherein, the viscosity of this low-viscosity cellulose mucus is 4000～7000 dregs of rice (poise).Wherein, the chemical constitution of this N-Methylol Caprolactom is as follows:
Advantage of the present invention is: wood pulp moistening ability height, reduced the mucus viscosity after the dissolving, and improve cellulosic dissolubility and spinnability and improved product quality, reduced cost.
Figure l is depicted as making process block diagram of the present invention.
Number in the figure is as follows:
1. the anti-polymerizations decline of surge tank 2. wood pulp celluloses 3. additives
4. mixed solvent 5. thin film evaporators 6. moisture content
7. low viscosity mucus
Now lift preferred embodiment and conjunction with figs. is described in detail as follows:
A kind of method for producing low-viscosity cellulose mucus of the present invention, it mainly is to be second solvent with N-Methylol Caprolactom (N-Methylol Caprolactom), and mix with certain proportion and to mix in the main solvent oxidation methyl woods (N-Methyl Morpholine Oxide), can in the process of dissolving, improve the splash humidity and the change solution composition of fiber, reach the effect that reduces cellulose mucus viscosity, and allow the processing procedure of solvent method can adopt dissolution in low temperature and high speed spinning, effectively solve the problem of commonly using the relevant cellulosic degree of polymerization decline of solvent method, and and then the rerum natura of reinforcing fiber product, improve the quality of products.
Because oxidation methyl woods (N-Methyl Morpholine Oxide) is for commonly using the solution of commonly using that solvent method adopted, therefore no longer add to give unnecessary details, but N-Methylol Caprolactom (N-MethylolCaprolactom) does not still have sale in the market, but its synthetic method is very simple and economical.
The synthesis step of N-Methylol Caprolactom is described below:
A. measure formaldehyde 32.6 grams of own interior vinegar amine (Caprolactom) 113 grams and 92%, in the reactor of a tool chuck, be heated to 70 ℃ of dissolvings;
B. the pH value with 0.1N NaOH (NaOH) adjustment reactant mixture is 11.0;
C. this reactor is with carbon dioxide (CO
2) gas is airtight, keeping temperature is 70 ± 5 ℃, 6 hours reaction time;
D. after reaction is finished, reactant mixture is shifted out this reactor, and be cooled to room temperature;
E. add the pure crystal seed of 1 gram standing over night after a day in this reactant mixture, get final product the white crystals of N-Methylol Caprolactoms of 140 grams.
The chemical constitution of this N-Methylol Caprolactom is as follows:
Major technique characteristics of the present invention are to reduce the viscosity of cellulose mucus, see also shown in Figure 1ly, and making flow process subitem of the present invention is described as follows:
The anti-polymerization decline additive 3 that in a surge tank 1, adds wood pulp cellulose 2 and 5000ppm (is benchmark with the wood pulp cellulose), and a mixed solvent 4; This mixed solvent 4 is to be mixed with about 7: 3 part by weight by oxidation methyl woods (70% weight ± 10%) and N-Methylol Caprolactom (30% weight ± 10%).With the wood pulp cellulose 2 of 46% weight mixed solvent 4,46% weight water and 8% weight and the mixture of this additive 3, in surge tank 1, evenly mixed 30 minutes jointly with 60 ℃, wood pulp fibre just can obtain sufficient Peng Run; Then the slurries of abundant Peng Run are sent in the thin film evaporator 5, under the condition of 90 ℃ temperature and 50～100mmHg decompression state about 5 minutes, just the moisture content 6 of slurries can be got rid of by 46% be 10%, forms low viscosity mucus 7.
Because the present invention has above-mentioned special making flow process and method, sees also the effect of utilizing mixed solvent shown in table one, table two and the table three, can use in the enforcement, produce following innovation effect:
(1) moistening ability height: the present invention's single solvent that the time ratio of Peng Run commonly uses of sizing mixing is short, and its need the quantity of bucket groove few, volume is little, can reduce the investment goods expense and improve solvability.
(2) mucus viscosity is low: the low-viscosity cellulose mucus that the present invention makes with mixed solvent, its viscosity is 4000～7000 dregs of rice (poise), under identical condition, its viscosity is low than single solvent, therefore can reduce by 5～10 ℃ of spinning temperatures, and and then reduce degree of polymerization fading rate 30% and reduce the solvent cracking raising rate of recovery 3～8%.
(3) reduce solvent cost: not on sale as yet on second solvent " N-Methylol Caprolactom " market that the present invention uses, but can utilize above-mentioned straightforward procedure to be synthesized, because synthetic cost is low, and it is about 20～40% to account for total solvent consumption ratio, so can reduce the cost of solvent.
(4) finished product rerum natura intensity height: the present invention reduces the viscosity of cellulose mucus, can improve the flowability and the extensibility of mucus, and improve spinning speed to more than the 1000M/min, the 100M/min of more traditional viscose process and the 400M/min that commonly uses solvent method are for high, not only can improve output, and because of finished product is the high speed spinning gained, the rerum natura intensity height of finished product.
Table one, moistening ability comparison sheet
| Solvent species | The cellulose kind | The profit of splashing condition (pH10.5) | Moistening ability (splash the profit before/Peng Run after) | The Peng Run ratio |
| Single oxidation methyl woods | Long fiber | 80℃*0.5Hr | 10-24/20-40μm | 1.7 |
| Single oxidation methyl woods | Staple fibre | 80℃*0.5Hr | 11-25/20-45μm | 1.8 |
| Solvent of the present invention | Long fiber | 80℃*0.5Hr | 10-24/25-45μm | 2.0 |
| Solvent of the present invention | Staple fibre | 80℃*0.5Hr | 11/25/25-50μm | 2.1 |
Table two, mucus viscosity comparison sheet
| Solvent species | Cellulosic degree of polymerization (DP) | Cellulose concentration | Solution temperature | Dissolving viscosity |
| Single oxidation methyl woods | 1050 | 12％ | 98℃ | 12000 poise |
| Solvent of the present invention | 1050 | 12％ | 98℃ | 6500poise |
Table three, solvent cost comparison sheet
| The solvent title | Unit price | Commonly use method | The present invention | ||
| Mixed proportion | Cost | Mixed proportion | Cost | ||
| The oxidation methyl woods | 270 yuan/kg | 100％ | 270 yuan/kg | 70％ | 189 yuan/kg |
| N-Methylol Caprolactom | 80 yuan/kg | - | - | 30％ | 24 yuan/kg |
| Close Meter | 270 yuan/kg | 213 yuan/kg | |||
Claims (3)
1. a method for producing low-viscosity cellulose mucus comprises the mixture of wood pulp fibre, mixed solvent and stabilization agent is dissolved into cellulose mucus through heating, reduce pressure, dewatering; It is characterized in that: this mixed solvent comprises the combined type solvent of main solvent oxidation methyl woods (N-Methyl Morpholine Oxide) and secondary solvent N-Methylol Caprolactom (N-Methylol Caprolactom), just, the mixed proportion of secondary solvent is 7 to 3; This mixed solvent total amount is 5.5～7.5 times of cellulose amount; This mixed solvent, when 12% cellulose mucus concentration, its viscosity is 6,500 dregs of rice (poise).
2. a kind of method for producing low-viscosity cellulose mucus according to claim 1, it is characterized in that: wherein, 46% weight mixed solvent, 46% weight water and 8% weight wood pulp cellulose, and with wood pulp cellulose weight be benchmark 5000ppm anti-polymerization decline additive in 60 ℃ mixed, evaporation removes moisture content to 10% weight in the mixed liquor that is obtained and forms this low-viscosity cellulose mucus.
3. a kind of method for producing low-viscosity cellulose mucus according to claim 2 is characterized in that: wherein, the viscosity of this low-viscosity cellulose mucus is 4000～7000 dregs of rice (poise).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN98101641A CN1084813C (en) | 1998-04-24 | 1998-04-24 | Method for producing low-viscosity cellulose mucus |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN98101641A CN1084813C (en) | 1998-04-24 | 1998-04-24 | Method for producing low-viscosity cellulose mucus |
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| Publication Number | Publication Date |
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| CN1195046A CN1195046A (en) | 1998-10-07 |
| CN1084813C true CN1084813C (en) | 2002-05-15 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN98101641A Expired - Fee Related CN1084813C (en) | 1998-04-24 | 1998-04-24 | Method for producing low-viscosity cellulose mucus |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN109337097B (en) * | 2018-10-29 | 2021-10-01 | 绍兴美标纺织品检验有限公司 | Solvent and method for preparing cellulose solution by using same |
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1998
- 1998-04-24 CN CN98101641A patent/CN1084813C/en not_active Expired - Fee Related
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