CN115992451A - Method for removing sodium sulfate attached to polyvinyl alcohol primary fiber - Google Patents

Method for removing sodium sulfate attached to polyvinyl alcohol primary fiber Download PDF

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Publication number
CN115992451A
CN115992451A CN202111218549.4A CN202111218549A CN115992451A CN 115992451 A CN115992451 A CN 115992451A CN 202111218549 A CN202111218549 A CN 202111218549A CN 115992451 A CN115992451 A CN 115992451A
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China
Prior art keywords
polyvinyl alcohol
sodium sulfate
treatment
hot water
fiber
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CN202111218549.4A
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Chinese (zh)
Inventor
王建
向鹏伟
冷平
徐小松
李会容
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China Petroleum and Chemical Corp
Sinopec Chongqing Chuanwei Chemical Co Ltd
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China Petroleum and Chemical Corp
Sinopec Chongqing Chuanwei Chemical Co Ltd
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Priority to CN202111218549.4A priority Critical patent/CN115992451A/en
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Abstract

The invention belongs to the technical field of separation, and particularly relates to a method for removing sodium sulfate attached to a polyvinyl alcohol primary fiber, which is to treat the polyvinyl alcohol primary fiber coming out of a coagulating bath with hot water at 30-60 ℃ and then squeeze the fiber. The method can effectively remove sodium sulfate attached to the primary fiber of the polyvinyl alcohol, and can also realize the recycling of the sodium sulfate.

Description

Method for removing sodium sulfate attached to polyvinyl alcohol primary fiber
Technical Field
The invention belongs to the technical field of separation, and particularly relates to a method for removing sodium sulfate attached to a polyvinyl alcohol nascent fiber.
Background
The polyvinyl alcohol fiber is a fiber produced from polyvinyl alcohol as a raw material, and is resistant to acids, alkali, mold and sunlight (chemical industry dictionary, chemical industry dictionary editorial, chemical industry Press, beijing: chemical industry Press, 1 st printing in 2003, 1286 pages, publication date 1 month 31 years 2003).
However, polyvinyl alcohol contains a large amount of hydroxyl groups, and the melting point (200 to 250 ℃) is close to the decomposition temperature, and melt spinning molding is difficult (research progress of modification method of melt processing of polyvinyl alcohol, fan Hua, etc., synthetic fiber, volume 35, 5 th, page 15, left column, 1 st paragraph, line 1 to 8, publication date; "current research status of melt processable polyvinyl alcohol", hou Shuangyan, etc., synthetic fiber, volume 38, 5, page 1, left column, 1 st to 5, publication date 2009, 12 months, 31).
At present, water is usually used as a solvent, sodium sulfate aqueous solution is used as a coagulating bath, and a wet spinning process is adopted to prepare the polyvinyl alcohol fiber ("wet spinning process discussion for preparing water-soluble PVA fiber", he Yun, synthetic fiber industry, volume 27, phase 4, page 32, right column, 2, line 1-10, publication date 2004, 12 months and 31).
However, after the coagulation bath treatment, about 20wt% to 30wt% sodium sulfate is attached to the nascent fiber.
Disclosure of Invention
In view of the above, an object of the present invention is to provide a method for removing sodium sulfate attached to a polyvinyl alcohol primary fiber.
In order to achieve the above purpose, the technical scheme of the invention is as follows:
the inventors have intensively studied to solve the above problems, and found that sodium sulfate attached to a polyvinyl alcohol primary fiber can be effectively removed by treating the polyvinyl alcohol primary fiber coming out of a coagulation bath with hot water of 30 to 60 ℃ and then squeezing the fiber.
Accordingly, one of the objects of the present invention is a method for removing sodium sulfate attached to a polyvinyl alcohol primary fiber, which comprises treating the polyvinyl alcohol primary fiber coming out of a coagulation bath with hot water at 30 to 60 ℃, and then squeezing the fiber.
The inventor finds that if the temperature of hot water is too low, sodium sulfate attached to nascent fibers cannot be effectively removed, and if the temperature of hot water is too high, fiber adhesion is easily caused.
The squeezing is a process of separating a liquid phase from a liquid-solid two-phase mixture (chemical industry dictionary, editorial, chemical industry Press, beijing: printing 1 st time of chemical industry press, 2003, page 267, publication date, 2003, 1 month, 31).
Preferably, the method comprises at least 2 cycles of hot water treatment-press treatment.
To further remove sodium sulfate attached to the primary fibers, the hot water is used in an amount of 0.5:1 to 1.5:1 mass ratio to the polyvinyl alcohol primary fibers coming out of the coagulation bath.
Preferably, the treatment comprises a spray treatment.
The invention also aims at protecting the production method of the polyvinyl alcohol fiber, which comprises the steps of solidification treatment and squeezing treatment, wherein the polyvinyl alcohol nascent fiber coming out of a solidification bath is treated by hot water at the temperature of 30-60 ℃, and then the fiber is squeezed.
To further remove sodium sulfate attached to the primary fibers, the hot water is used in an amount of 0.5:1 to 1.5:1 mass ratio to the polyvinyl alcohol primary fibers coming out of the coagulation bath.
Preferably, the treatment comprises a spray treatment.
Preferably, the production process comprises at least 2 cycles of hot water treatment-press treatment.
Preferably, the press liquid obtained by the press treatment is used as the coagulation bath replenishing liquid.
The invention has the beneficial effects that:
the invention uses 30-60 ℃ hot water to treat, then presses the fiber, thereby effectively removing sodium sulfate attached to the polyvinyl alcohol nascent fiber.
The invention adopts hot water to recycle sodium sulfate in the polyvinyl alcohol nascent fiber, the obtained recycling liquid has high solute content, and can be used as a supplementary liquid of the coagulating bath to enter the coagulating bath for recycling, thereby not only reducing the production cost, but also reducing the environmental pollution.
Detailed Description
The examples are presented for better illustration of the present invention, but are not intended to limit the scope of the present invention to the examples. Those skilled in the art will appreciate that various modifications and adaptations of the embodiments described above are possible in light of the above teachings and are intended to be within the scope of the invention.
The following sodium sulfate content detection method comprises the following steps:
instrument: analytical balance with an accuracy of 0.1mg; a muffle furnace;
the test steps are as follows: after fully and uniformly mixing the samples, weighing 2-5g of samples; placing the sample into a porcelain crucible with constant weight, moving the porcelain crucible into an oven, and drying the porcelain crucible at 110 ℃ until the weight is constant; taking out, cooling to room temperature in a dryer, and weighing; carefully carbonizing in an electric furnace, then transferring into a muffle furnace, and burning to constant weight at 750-800 ℃; taken out, cooled to room temperature in a dryer and weighed.
Sodium sulfate (Na) 2 SO 4 ) The content is expressed as mass fraction X 1 Values are expressed as percent%; calculated according to the following formula:
Figure BDA0003311642350000021
wherein:
X 1 sodium sulfate (Na) 2 SO 4 ) Numerical values of the content in percent (%); m is m 1 The mass of the ceramic crucible is given as a numerical value, and the unit is gram (g);
m 2 the unit is gram (g) which is the numerical value of the mass of the dried sample and the porcelain crucible; m is m 3 The unit is gram (g) which is the numerical value of the mass of the sample and the porcelain crucible after firing;
sodium sulfate (Na) 2 SO 4 ) The content is expressed as the arithmetic mean of the results of two parallel experiments.
Example 1
The method for removing sodium sulfate attached to polyvinyl alcohol fibers comprises the following steps:
after being treated by a wet-heat coagulation bath (sodium sulfate solution), the primary fiber of polyvinyl alcohol (before being treated) is attached with about 25 percent sodium sulfate, and the primary fiber yarn bundle is subjected to spray treatment (the water spraying amount is about 1/2 of the mass of the yarn bundle) by hot water at 45 ℃, and then is subjected to squeezing treatment;
then, the tow is subjected to secondary spraying treatment (the water spraying amount is about 1/2 of the mass of the tow) by hot water at 45 ℃ again, and then the tow is subjected to secondary squeezing treatment;
and recovering the squeeze liquid obtained by the twice squeezing treatment and collecting the squeeze liquid together, wherein the squeeze liquid is taken as a coagulating bath supplementary liquid to enter the coagulating bath for recycling.
Performance detection
The sodium sulfate content of the tow after the second press in example 1 was measured and the results are shown in table 1.
TABLE 1 Performance test results
Source Sodium sulfate content of the nascent fiber before treatment Sodium sulfate content of tow after secondary squeezing/wt%
Example 1 24.8 7.0
Furthermore, it should be understood that although the present disclosure describes embodiments, not every embodiment is provided with a separate embodiment, and that this description is provided for clarity only, and that the disclosure is not limited to the embodiments described in detail below, and that the embodiments described in the examples may be combined as appropriate to form other embodiments that will be apparent to those skilled in the art.

Claims (7)

1. A method for removing sodium sulfate attached to primary polyvinyl alcohol fibers, characterized by: the primary fibres of polyvinyl alcohol coming out of the coagulation bath are treated with hot water at 30-60 ℃ and subsequently pressed.
2. The method of claim 1, comprising at least 2 cycles of hot water treatment-press treatment.
3. The method according to claim 1 or 2, characterized in that the total amount of hot water is 0.5:1-1.5:1 by mass to the primary fibres of polyvinyl alcohol coming out of the coagulation bath.
4. A method according to any one of claims 1-3, wherein the treatment comprises a spray treatment.
5. A process for preparing polyvinyl alcohol fibres includes such steps as coagulating and squeezing, and features that the primary polyvinyl alcohol fibres coming out of coagulating bath are treated by 30-60 deg.C hot water, and then squeezing.
6. The method of claim 5, comprising at least 2 cycles of hot water treatment-press treatment.
7. The method according to claim 5 or 6, wherein the press liquid obtained by the press treatment is recycled as the coagulation bath replenishing liquid.
CN202111218549.4A 2021-10-20 2021-10-20 Method for removing sodium sulfate attached to polyvinyl alcohol primary fiber Pending CN115992451A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202111218549.4A CN115992451A (en) 2021-10-20 2021-10-20 Method for removing sodium sulfate attached to polyvinyl alcohol primary fiber

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202111218549.4A CN115992451A (en) 2021-10-20 2021-10-20 Method for removing sodium sulfate attached to polyvinyl alcohol primary fiber

Publications (1)

Publication Number Publication Date
CN115992451A true CN115992451A (en) 2023-04-21

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