CN111544954A - Coagulating bath purification treatment method for producing flame-retardant viscose fibers - Google Patents

Coagulating bath purification treatment method for producing flame-retardant viscose fibers Download PDF

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Publication number
CN111544954A
CN111544954A CN202010455604.0A CN202010455604A CN111544954A CN 111544954 A CN111544954 A CN 111544954A CN 202010455604 A CN202010455604 A CN 202010455604A CN 111544954 A CN111544954 A CN 111544954A
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treatment method
coagulating bath
filtration
retardant viscose
filter
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Inventor
马君志
王成涛
刘长军
葛红
李昌垒
刘乐
吴亚红
秦翠梅
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Weifang Xinlong Biomaterials Co Ltd
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Weifang Xinlong Biomaterials Co Ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D36/00Filter circuits or combinations of filters with other separating devices
    • B01D36/02Combinations of filters of different kinds
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D36/00Filter circuits or combinations of filters with other separating devices
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D37/00Processes of filtration
    • B01D37/02Precoating the filter medium; Addition of filter aids to the liquid being filtered
    • B01D37/025Precoating the filter medium; Addition of filter aids to the liquid being filtered additives incorporated in the filter

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Filtration Of Liquid (AREA)
  • Filtering Materials (AREA)

Abstract

The invention provides a coagulating bath purification treatment method for producing flame-retardant viscose fibers. The acid bath purification treatment method can remove the impurities such as sulfide, hemicellulose, ash colloid blocks and the like in the acid bath, and can also remove silicon dioxide colloid, the transparency of the acid bath is greatly improved, the content of the silicon dioxide colloid in the acid bath is reduced from 0.3-0.4g/L to less than 0.02g/L, the transparency is improved from less than or equal to 30mm to more than or equal to 1000mm, and the appearance is improved from milk white to colorless and transparent; the acid bath purification treatment method of the invention keeps the concentration of sulfuric acid, zinc sulfate and sodium sulfate in the acid bath components constant before and after treatment.

Description

Coagulating bath purification treatment method for producing flame-retardant viscose fibers
Technical Field
The invention relates to a treatment method for purifying and recycling a coagulating bath in the viscose fiber production field, in particular to a technological method for purifying and treating the coagulating bath in the production of silicon flame-retardant viscose fibers, belonging to the technical field of viscose fibers.
Background
A series of reactions are generated in the viscose spinning forming process, and impurities such as sulfide, colloidal sulfur, semi-fiber and ash brought by viscose and colloidal lumps generated in the forming process enter a coagulating bath, so that the coagulating bath becomes turbid, and the normal spinning is influenced. The acid bath filter is the main equipment for filtering solid impurities in the acid bath, and mainly goes through different periods of quartz sand filters, microporous filters, polypropylene tow filters and the like. Chinese patent CN201410366656 discloses a method for removing solid impurities in acid bath, which adopts 200-mesh filter cloth, has pressure of 0.5Mpa, and uses a plate-and-frame filter to treat solid impurities contained in common viscose fiber acid bath. Patent CN201721442689 designs a set of micro-pore filter small-sized acid bath filtration backwashing system; in the production of polynosic fiber, a diatomite filter is adopted in order to meet the requirement of a high-transparency coagulating bath in the Dandong chemical fiber factory, and a vacuum filter pre-coated with diatomite is adopted in the patent CN201711155675 to treat the dipping alkali liquor. Although the diatomite filter greatly improves the filtering precision, the filtering efficiency is reduced.
Patent CN201210065248 discloses a flame-retardant silicate fiber, a coagulating bath for producing the flame-retardant silicate fiber and a method for preparing the flame-retardant silicate fiber, wherein the forming coagulating bath of the silicate fiber contains H2SO4、ZnSO4、Na2SO4And soluble SiO2. The purifying treatment and the recycling of the coagulating bath in the production process of the silicon-based flame-retardant viscose fiber are more complicated compared with the common viscose, and the crystal substances of which the main components are polysilicic acid and sodium sulfate can be known through the analysis of the filtration and interception substances of the polypropylene tow filterThe substance is adhered to the polypropylene fiber tow to form a 'filter layer', and acid mud in the coagulating bath quickly covers the adhered substance, so that the traditional filter loses the filtering capability, impurities cannot be removed in time, the circulation system of the acid bath is seriously blocked, and the process is unstable. The spinnability of the spinning becomes worse and the defects are obviously increased. The polypropylene fiber tow filter and various impurity components are mixed, selective filtration cannot be realized, tows are rapidly bonded into a bundle shape, the filtration effect is lost, and a series of problems of high equipment failure rate, high maintenance cost, high environmental protection treatment cost, high bath amount loss and the like of filter flash evaporation and the like are caused. If the diatomite filter is directly adopted, various impurities are rapidly accumulated on the diatomite coating, the pressure is increased, the coating is frequently replaced, the efficiency is low, the cost is high, and the acid bath loss is serious. No data report exists so far aiming at the successful treatment of the silicon-containing coagulating bath in the production of silicon-based flame-retardant fibers.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a coagulating bath purification treatment method for producing flame-retardant viscose fibers, which realizes the following purposes:
the content of silicon dioxide colloid in the acid bath is reduced, and the transparency of the acid bath is improved; while not affecting the concentration of the acid bath components.
In order to solve the technical problems, the invention adopts the following technical scheme:
a coagulating bath purification treatment method for producing flame-retardant viscose fibers comprises primary filtration and fine filtration.
The following is a further improvement of the above technical solution:
the processing method specifically comprises the following steps:
1. preliminary filtration
1.1 filtration of solid impurities in the coagulation bath: pumping the degassed waste acid bath into a plate and frame filter from a waste acid tank by using an acid bath circulating pump, intercepting solid impurities by using polypropylene felts or double-faced velvet on the filter plate to realize solid-liquid separation, and allowing the filtered acid bath to enter a fine filtering process, wherein acid mud is accumulated between the filter plates.
The filter material is polypropylene felt or double-faced velvet;
the specification of the polypropylene fiber felt is 1100-1300 g/m2Preferably 1100g/m2Or 1300g/m2
The specification of the double-sided velvet is 75-85 s-2Preferably 80 s-2
1.2 solid impurity removal: when the inlet pressure of the plate-frame filter reaches 0.4MPa, the feeding is stopped. The pressurizing device raises the pressure of the filter plate to 0.55MPa, and the acid bath is extruded from the acid mud and enters the production system. The sludge enters a production garbage field for treatment.
1.3 coagulation bath composition comparison
Figure 47003DEST_PATH_IMAGE001
After primary filtration, the transparency is preferably 25-30 mm, and is increased to 40-50 mm;
the components of the acid bath, such as sulfuric acid, zinc sulfate, sodium sulfate and silicon dioxide, are not changed, the transparency of the acid bath is slightly improved, but impurities, such as sulfide, hemicellulose, ash colloid blocks and the like, are removed.
2. Fine filtration
2.1 using the flame-retardant acid bath after coarse filtration, respectively preparing pre-paving mother liquor with different amounts, types and contents of diatomite, and uniformly stirring.
2.2 start the filter feed pump and pre-coat the fine filter with diatomaceous earth in a coarse filter acid bath to which diatomaceous earth is added.
Pre-coating film amount: 500-1200 g/m2Pre-coating working pressure: 0.2-0.35 Mpa, preferably 0.3-0.35Mpa, diatomaceous earth: AG-100#、AG-500#、 AG-700#Or mixtures thereof.
2.3 the coating is finished, the valve is switched, the coarse filtration coagulating bath is subjected to fine filtration, and the working pressure of filtration is as follows: less than 0.4 Mpa; the filter base cloth filter material is polypropylene fiber felt or double-faced flannelette, and the specification of the polypropylene fiber felt is 1100-plus-material 1300g/m2The specification of the double-sided velvet is 75-85s2
The filter used for fine filtration is a plate and frame filter.
2.4 after the filtration pressure is increased, the feeding valve is closed, the filtrate is emptied, and the diatomite filter residue containing the orthosilicic acid is discharged. Then, the pre-coating process is performed.
2.5 the coagulating bath after fine filtration directly enters into flash evaporation for evaporation, and a part of the acid bath after evaporation enters into a crystallizer and a part of the acid bath is supplied to a production system, so that stable operation of production is met.
2.6 coagulation bath composition comparison
Figure 782878DEST_PATH_IMAGE002
After fine filtration, SiO2The content is reduced to 0.01-0.018 g/L; the transparency is improved to 1000-1200 mm;
the components of the acid bath, namely sulfuric acid, zinc sulfate and sodium sulfate are not changed, but the silicon dioxide colloid in the acid bath is greatly reduced, the transparency of the acid bath is greatly improved, and the acid bath is purified.
Aiming at the complex impurity components such as inorganic salt, solid particles, colloidal substances and the like existing in the flame-retardant viscose fiber coagulation bath, the invention removes the impurities such as sulfide, colloidal sulfur, semi-fiber, ash colloidal mass and the like in order to retain the components beneficial to spinning forming. Providing a plate-and-frame filter which takes a plate-and-frame filter as a carrier and uses polypropylene fiber felt and double-faced velvet as filter materials for primary filtration to remove impurities such as hemicellulose, acid mud, polysulfide and the like through filtration; the fine filtration adopts diatomite to pre-coat the filter material, and then filtration treatment is carried out to remove the silicic acid in a colloidal state, so as to obtain high-purity coagulation bath components, and realize the purification, recovery and cyclic utilization of the coagulation bath.
Compared with the prior art, the invention has the following technical effects:
(1) the acid bath purification treatment method can remove the impurities such as sulfide, hemicellulose, ash colloid blocks and the like in the acid bath, and can also remove silicon dioxide colloid, the transparency of the acid bath is greatly improved, the content of the silicon dioxide colloid in the acid bath is reduced from 0.3-0.4g/L to less than 0.02g/L, the transparency is improved from less than or equal to 30mm to more than or equal to 1000mm, and the appearance is improved from milk white to colorless and transparent.
(2) The acid bath purification treatment method of the invention keeps the concentration of sulfuric acid, zinc sulfate and sodium sulfate in the acid bath components constant before and after treatment.
(3) Aiming at the characteristics of components of a coagulation bath produced by the silicon-based flame-retardant viscose, a graded continuous filtering mode is invented for selectively filtering impurity components in the coagulation bath and improving the filtering capacity and the filtering effect by means of a plate-and-frame filter form with high automation degree and good production environment, preferably selecting a proper filter material and exploring the filtering process conditions. Is a low-cost, easy-to-operate acid bath purification treatment method which is particularly suitable for the production of silicon flame-retardant fibers.
Detailed Description
The invention is further described with reference to specific examples. The examples merely represent one embodiment of the invention and are not to be construed as limiting the scope of the invention.
Example 1
1. Coarse filtration
Pumping the degassed waste acid bath circulating pump into a plate-and-frame filter from a waste acid tank, wherein the filter material is polypropylene fiber felt 1100g/m2The working pressure of the inlet of the filter is 0.4Mpa, and sampling analysis is carried out. Colloidal polysulphides and organic semi-fibrous matter can be found in the filter sludge. The compositions before and after coagulation bath filtration are compared as follows.
Figure 309674DEST_PATH_IMAGE003
The components of the coagulating bath, namely sulfuric acid, zinc sulfate, sodium sulfate and silicon dioxide, are slightly changed and are approximately unchanged, the transparency of the acid bath is slightly improved, but impurities such as sulfide, hemicellulose, ash colloid blocks and the like are removed.
2. Fine filtration
The coagulation bath after the rough filtration treatment was introduced from the acid pipe into a filter to be precoated with diatomaceous earth.
The base cloth filter material of the fine filter is 1300g/m2Polypropylene felt, precoating amount: 500 g/m2Pre-coating working pressure: 0.35Mpa, diatomaceous earth: AG-100#And filtering working pressure: sampling at 3.9MPa for analysis. The components before and after the coagulation bath essence filtration are compared asThe following steps.
Figure 447394DEST_PATH_IMAGE004
The components of the coagulating bath, namely sulfuric acid, zinc sulfate and sodium sulfate are not changed approximately, soluble silicon dioxide is removed, and the transparency of the acid bath is improved to 1200 mm. The coagulation bath became transparent and clear.
Example 2
1. Pumping the degassed waste acid bath into a plate-and-frame filter from a waste acid tank by an acid bath circulating pump for coarse filtration, wherein the polypropylene fiber felt on the filter plate is 1300g/m2Solid impurities are intercepted, solid-liquid separation is realized, and acid sludge is accumulated between filter plates. Removal of acid bath from solid impurities: and when the inlet pressure of the plate-frame filter reaches 0.4MPa, sampling and analyzing, and stopping feeding. The pressurizing device raises the pressure of the filter plate to 0.55MPa, and the acid bath is extruded from the acid mud and enters the production system. The sludge enters a production garbage field for treatment, and colloidal polysulfide and organic hemicellulose substances can be found in the filter residue sludge. The compositions before and after coagulation bath filtration are compared as follows.
Figure 519386DEST_PATH_IMAGE005
The components of the coagulating bath, namely sulfuric acid, zinc sulfate, sodium sulfate and silicon dioxide, are slightly changed and are approximately unchanged, and the transparency of the acid bath is slightly improved.
2. The coagulation bath for coarse filtration was fed from the acid pipe and subjected to fine filtration through a precoated diatomaceous earth filter. The base cloth filter material of the fine filter is 1300g/m2Polypropylene felt, precoating amount: 800 g/m2Pre-coating working pressure: 0.3 Mpa, diatomaceous earth: AG-700#And filtering working pressure: sampling at 3.5MPa for analysis. The compositions before and after coagulation bath filtration are compared as follows.
Figure 601612DEST_PATH_IMAGE006
The components of the coagulating bath, namely sulfuric acid, zinc sulfate and sodium sulfate are not changed approximately, soluble silicon dioxide is removed, and the transparency of the acid bath is improved to 1100 mm. The coagulation bath became transparent and clear.
Example 3
1. Pumping the degassed waste acid bath into a plate-and-frame filter from a waste acid tank by using an acid bath circulating pump, and collecting 80s on a filter plate2Solid impurities are intercepted by the double-sided velvet, solid-liquid separation is realized, and acid mud is accumulated between the filter plates. Removal of acid bath from solid impurities: and when the inlet pressure of the plate-frame filter reaches 0.4MPa, stopping feeding, and sampling and analyzing. The pressurizing device raises the pressure of the filter plate to 0.55MPa, and the acid bath is extruded from the acid mud and enters the production system. The sludge enters a production garbage field for treatment, and colloidal polysulfide and organic hemicellulose substances can be found in the filter residue sludge. The compositions before and after coagulation bath filtration are compared as follows.
Figure 933366DEST_PATH_IMAGE007
The components of the coagulating bath, namely sulfuric acid, zinc sulfate, sodium sulfate and silicon dioxide, are slightly changed and are approximately unchanged, and the transparency of the acid bath is slightly improved.
2. The coagulation bath after the coarse filtration was passed from the acid tube into a filter precoated with diatomaceous earth for fine filtration. The base cloth filter material of the fine filter is 1100g/m2Polypropylene felt, precoating amount: 1000 g/m2Pre-coating working pressure: 0.3 Mpa, diatomaceous earth: AG-100#And AG-700#Mixture, ratio 1:1, filtration working pressure: sampling at 3.5MPa for analysis. The compositions before and after coagulation bath filtration are compared as follows.
Figure 925592DEST_PATH_IMAGE008
The components of the coagulating bath, namely sulfuric acid, zinc sulfate and sodium sulfate are not changed approximately, soluble silicon dioxide is removed, and the transparency of the acid bath is improved to 1000 mm. The coagulation bath became transparent and clear.
Example 4
1. Coarse filtration
Pumping the degassed waste acid bath circulating pump into a plate-and-frame filter from a waste acid tank, wherein the filter material is selectedPolypropylene felt 1300g/m2The working pressure of the inlet of the filter is 0.4Mpa, and sampling analysis is carried out. Colloidal polysulphides and organic semi-fibrous matter can be found in the filter sludge. The compositions before and after coagulation bath filtration are compared as follows.
Figure 683333DEST_PATH_IMAGE009
The components of the coagulating bath, namely sulfuric acid, zinc sulfate, sodium sulfate and silicon dioxide, are slightly changed and are approximately unchanged, the transparency of the acid bath is slightly improved, but impurities such as sulfide, hemicellulose, ash colloid blocks and the like are removed.
2. Fine filtration
The coagulation bath after the rough filtration treatment was introduced from the acid pipe into a filter to be precoated with diatomaceous earth.
The base cloth filter material of the fine filter is 1300g/m2Polypropylene felt, precoating amount: 1200 g/m2Pre-coating working pressure: 0.35Mpa, diatomaceous earth: AG-100#And AG-500#Mixture, ratio 1:2, filtration operating pressure: sampling at 3.9MPa for analysis. The compositions before and after coagulation bath filtration are compared as follows.
Figure 393800DEST_PATH_IMAGE010
The components of the coagulating bath, namely sulfuric acid, zinc sulfate and sodium sulfate are not changed approximately, soluble silicon dioxide is removed, and the transparency of the acid bath is improved to 1200 mm. The coagulation bath became transparent and clear.

Claims (9)

1. A coagulating bath purification treatment method for producing flame-retardant viscose fibers is characterized by comprising the following steps: the treatment method comprises primary filtration and fine filtration.
2. The coagulating bath purifying treatment method for producing flame-retardant viscose fiber according to claim 1, wherein: and in the fine filtration, the filter is precoated with diatomite and then fine filtration is carried out.
3. The coagulating bath purifying treatment method for producing the flame-retardant viscose fiber according to claim 2, wherein: the precoating diatomite has a precoating film amount of 500-1200 g/m2Pre-coating working pressure: 0.2-0.35 Mpa.
4. The coagulating bath purifying treatment method for producing the flame-retardant viscose fiber according to claim 2, wherein: the diatomite is AG-100#、AG-500#、 AG-700#One or more of (a).
5. The coagulating bath purifying treatment method for producing flame-retardant viscose fiber according to claim 1, wherein: and fine filtering, wherein the filtering working pressure is less than 0.4 Mpa.
6. The coagulating bath purifying treatment method for producing flame-retardant viscose fiber according to claim 1, wherein: and (3) filtering by adopting a plate-and-frame filter for primary filtering, and stopping feeding when the inlet pressure reaches 0.4 MPa.
7. The coagulating bath purifying treatment method for producing flame-retardant viscose fiber according to claim 1, wherein: the filter base cloth filter materials adopted in the primary filtration and the fine filtration are polypropylene felts or double-faced flannelette;
the specification of the polypropylene fiber felt is 1100-1300 g/m2The specification of the double-sided velvet is 75-85s2
8. The coagulating bath purifying treatment method for producing flame-retardant viscose fiber according to claim 1, wherein: the impurities removed by the primary filtration comprise sulfides, semi-fibers and ash gel blocks; the transparency of the coagulating bath after the initial filtration is improved to 30-50mm from less than or equal to 30 mm.
9. The coagulating bath purifying treatment method for producing flame-retardant viscose fiber according to claim 1, wherein: the content of silicon dioxide in the coagulating bath is reduced from 0.3-0.4g/L to less than 0.02g/L by fine filtration; the transparency is improved from 30-50mm to more than or equal to 1000 mm.
CN202010455604.0A 2020-05-26 2020-05-26 Coagulating bath purification treatment method for producing flame-retardant viscose fibers Withdrawn CN111544954A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114606585A (en) * 2020-12-03 2022-06-10 中国石油化工股份有限公司 Method for improving transparency of coagulation bath

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114606585A (en) * 2020-12-03 2022-06-10 中国石油化工股份有限公司 Method for improving transparency of coagulation bath

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