CN112408431B - Method for preparing anhydrous sodium sulphate by acid bath evaporation of viscose - Google Patents
Method for preparing anhydrous sodium sulphate by acid bath evaporation of viscose Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D5/00—Sulfates or sulfites of sodium, potassium or alkali metals in general
- C01D5/006—Recovery of sodium sulfate from coagulation baths for the spinning of viscose
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Abstract
The invention relates to the technical field of viscose fiber production, in particular to a method for preparing anhydrous sodium sulphate by viscose fiber acid bath evaporation. The method for preparing anhydrous sodium sulphate by viscose acid bath evaporation comprises the following steps: carrying out first reduced pressure evaporation on the acid bath pretreatment liquid, carrying out first cooling crystallization, and filtering to obtain a sodium sulfate decahydrate crude product; redissolving the crude sodium sulfate decahydrate with water to obtain a sodium sulfate redissolution, adding a newly prepared active carbon hydrogen peroxide treatment solution into the sodium sulfate redissolution, heating, stirring and filtering to obtain a sodium sulfate purified solution; carrying out secondary reduced pressure evaporation on the sodium sulfate purified solution, carrying out secondary cooling crystallization, and washing crystals with a saturated sodium sulfate solution to obtain a pure sodium sulfate decahydrate product; and drying the pure sodium sulfate decahydrate to obtain anhydrous sodium sulphate. The anhydrous sodium sulphate prepared by the method has higher purity and whiteness, and lower zinc content and water-insoluble substance content.
Description
Technical Field
The invention relates to the technical field of viscose fiber production, in particular to a method for preparing anhydrous sodium sulphate by viscose fiber acid bath evaporation.
Background
The viscose fiber acid bath mainly comprises a solution prepared from sulfuric acid, sodium sulfate and zinc sulfate, and can be used for solidifying and spinning viscose, which is an important step in viscose fiber production, the content of each component in the acid bath, the clarity and cleanliness of the solution, the temperature and the like are critical to the quality of the viscose fiber, a large amount of sulfuric acid is consumed in the acid bath process of the viscose fiber to generate sodium sulfate, the sodium sulfate can be separated out on the viscose fiber after saturation is achieved, the solidification time of the viscose is influenced, and the viscose solidification bath can bring impurities such as sulfides, short fibers, glue blocks and the like to cause turbidity of the solution, so that the viscose acid bath needs to be recycled to remove excessive water, sodium sulfate and impurities. Acid bath evaporation is a method for removing redundant sodium sulfate and water which are frequently used in the prior art, anhydrous sodium sulphate can be prepared by the method, and in the prior art, no purification step is involved in the preparation process of the anhydrous sodium sulphate, so that water-insoluble impurities such as zinc sulfate, cellulose, sulfur-containing substances and the like are mixed in the recovered anhydrous sodium sulphate, and the product purity is poor.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a method for preparing anhydrous sodium sulphate by acid bath evaporation of viscose fibers.
The technical scheme adopted by the invention for solving the technical problem is to provide a method for preparing anhydrous sodium sulphate by viscose acid bath evaporation, which comprises the following steps:
1) Pretreatment: carrying out aeration and filtration pretreatment on an acid bath for viscose spinning to obtain an acid bath pretreatment solution;
2) Primary evaporation and crystallization: carrying out first reduced pressure evaporation on the acid bath pretreatment liquid, carrying out first cooling crystallization, and filtering to obtain a sodium sulfate decahydrate crude product;
3) Redissolving and purifying: redissolving the crude sodium sulfate decahydrate with water to obtain a sodium sulfate redissolution, adding a newly prepared active carbon hydrogen peroxide treatment solution into the sodium sulfate redissolution, heating, stirring and filtering to obtain a sodium sulfate purified solution;
4) And (3) recrystallization: carrying out secondary reduced pressure evaporation on the sodium sulfate purified solution, carrying out secondary cooling crystallization, and washing crystals with a saturated sodium sulfate solution to obtain a pure sodium sulfate decahydrate product;
5) And (3) drying: and drying the pure sodium sulfate decahydrate product to obtain anhydrous sodium sulfate.
The recovery of sodium sulfate in the acid bath recovery can not only reduce the concentration of sodium sulfate in the acid bath, but also can produce anhydrous sodium sulfate. The sodium sulfate in the acid bath is prepared by adopting a conventional primary purification and crystallization method, impurities such as zinc sulfate, water-insoluble cellulose and sulfides can be mixed in the obtained sodium sulfate, the purity and whiteness of the prepared anhydrous sodium sulphate are low due to the existence of the substances, and the impurities such as the cellulose and the sulfides contained in the anhydrous sodium sulphate are easy to agglomerate, so that the granularity, the granularity and the whiteness of the anhydrous sodium sulphate are poor. In order to improve whiteness and reduce impurities such as cellulose, sulfide and the like, the prior art usually adopts high temperature of over 800 ℃ for roasting, which needs to consume a large amount of heat energy and pollutes the atmosphere. In the invention, sodium sulfate obtained by crystallization is redissolved and purified by selecting the active carbon hydrogen peroxide treatment liquid, on one hand, the applicant finds that hydrogen peroxide can improve the adsorption capacity of active carbon on water-insoluble impurities and zinc in anhydrous sodium sulphate, and the anhydrous sodium sulphate has higher purity. On the other hand, the hydrogen peroxide can oxidize the low-valence sulfide in the sulfide sodium sulfate redissolution into sulfur, and the sulfur-containing impurities in the anhydrous sodium sulfate are removed by a filtering method.
In addition, the invention sets the steps of redissolution purification and recrystallization, the pH value of the sodium sulfate redissolution is obviously improved and is close to neutrality compared with that of an acid bath, zn & lt 2+ & gt begins to precipitate under the condition, the settling speed of Zn & lt 2+ & gt is accelerated in the presence of the activated carbon hydrogen peroxide treatment solution in the solution, and the zinc content of the finally obtained anhydrous sodium sulphate is lower.
Further, the active carbon hydrogen peroxide solution treatment liquid in the step 3) is 10-15% of the volume of the sodium sulfate redissolution solution.
Further, the preparation method of the active carbon hydrogen peroxide solution in the step 3) comprises the steps of adding the active carbon into the hydrogen peroxide solution, and stirring for 20-30min at 50-60 ℃ to obtain the active carbon hydrogen peroxide solution.
Further, the concentration of the hydrogen peroxide solution is 30-40%, and the mass ratio of the activated carbon to the hydrogen peroxide solution is 2-4.
Furthermore, the activated carbon is coconut shell activated carbon with the particle size of 0.4-3 mm.
Further, the temperature of the first decompression evaporation in the step 2) is 60-70 ℃, and the vacuum degree is 2 x 10 4 Pa—8×10 4 Pa；
And/or the first reduced pressure evaporation is concentrated to 1/2-3/4 of the volume of the pretreatment liquid of the acid bath;
and/or the temperature of the first cooling crystallization in the step 2) is 15-20 ℃.
Further, the mass concentration of sodium sulfate in the redissolution solution in the step 3) is 35-40%; and/or the temperature of the reconstitution is 40-50 ℃.
Further, the heating and stirring in the step 3) are carried out for 30-40min at the temperature of 40-50 ℃ and at the speed of 300-500 rpm/min.
Further, the temperature of the second reduced pressure evaporation in the step 4) is 60-70 ℃, and the vacuum degree is 2 x 10 4 Pa—8×10 4 Pa；
And/or the second reduced pressure evaporation in the step 4) needs to be concentrated to 3/5-3/4 of the volume of the sodium sulfate purified liquid;
and/or the second cooling crystallization temperature in the step 4) is firstly cooled to 40-50 ℃, and is kept for 20-30min; then cooling to 15-20 ℃ for crystallization until crystallization is complete.
Further, the drying in the step 5) is carried out for 12-14h at 120-150 ℃.
Compared with the prior art, the invention has the following beneficial effects: the anhydrous sodium sulphate is redissolved and purified by using the active carbon hydrogen peroxide treatment solution; on the one hand, the applicant finds that the hydrogen peroxide can improve the adsorption capacity of the activated carbon on water-insoluble impurities and zinc in the anhydrous sodium sulphate, and the anhydrous sodium sulphate is higher in purity. On the other hand, the hydrogen peroxide can oxidize the low-valence sulfide in the sodium sulfide redissolution into sulfur, and remove sulfur-containing impurities in the anhydrous sodium sulphate by a filtering method.
Detailed Description
The experimental procedures in the following examples are conventional unless otherwise specified. The raw materials in the following examples are all commercially available products and are commercially available, unless otherwise specified. The present invention is described in further detail below with reference to examples:
example 1
The embodiment provides a method for preparing anhydrous sodium sulphate by viscose acid bath evaporation, which comprises the following steps:
1) Pretreatment: carrying out acid bath aeration treatment on the viscose for viscose spinning to remove most of sulfide in the viscose, and filtering to remove most of cellulose and solid impurities to obtain acid bath pretreatment liquid;
2) Primary evaporation and crystallization: acid bath pretreatment solution was heated at 65 ℃ under a vacuum of 4X 10 4 Carrying out first reduced pressure evaporation under Pa until the volume is 1/2 of the original volume; then crystallizing for 3h at 18 ℃, and filtering to obtain a sodium sulfate decahydrate crude product;
3) Redissolving and purifying: adding water into a sodium sulfate decahydrate crude product, dissolving at 45 ℃ to prepare a sodium sulfate redissolution with the mass concentration of 38%, adding a newly prepared activated carbon hydrogen peroxide treatment solution with the volume of 15% of the sodium sulfate redissolution into the sodium sulfate redissolution (wherein the preparation method of the activated carbon hydrogen peroxide solution is to add activated carbon into a 35% hydrogen peroxide solution, stirring at 55 ℃ for 25min to obtain the sodium sulfate purified solution, wherein the mass ratio of the activated carbon to the hydrogen peroxide solution is 3, and the activated carbon is coconut shell activated carbon with the particle size of 0.4-3 mm), stirring at 45 ℃ and 400rpm/min for 35min, and filtering to obtain the sodium sulfate purified solution;
4) And (3) recrystallization: sodium sulfate purified solution at 65 deg.C and vacuum degree of 4 × 10 4 Carrying out second reduced pressure evaporation under Pa to 3/4 of the original volume, cooling to 45 ℃, and keeping for 25min; then cooling to 18 ℃ for crystallization for 5h, and washing the obtained crystal with a saturated sodium sulfate solution to obtain a pure sodium sulfate decahydrate product;
5) And (3) drying: drying the pure sodium sulfate decahydrate at 135 ℃ for 13h to obtain anhydrous sodium sulfate.
Example 2
The embodiment provides a method for preparing anhydrous sodium sulphate by viscose acid bath evaporation, which comprises the following steps:
1) Pretreatment: carrying out aeration treatment on an acid bath for viscose spinning to remove most of sulfide in the acid bath, and filtering to remove most of cellulose and solid impurities to obtain an acid bath pretreatment solution;
2) Primary evaporation and crystallization: the acid bath pretreatment liquid was heated at 60 ℃ under a vacuum of 2X 10 4 Concentrating under Pa to 3/4 of the original volume; then crystallizing for 2 hours at 15 ℃, and filtering to obtain a sodium sulfate decahydrate crude product;
3) Redissolving and purifying: adding water into a sodium sulfate decahydrate crude product, dissolving at 45 ℃ to prepare a sodium sulfate redissolution with the mass concentration of 40%, adding a newly prepared activated carbon hydrogen peroxide treatment solution with the volume of 13% of the sodium sulfate redissolution into the sodium sulfate redissolution (wherein the preparation method of the activated carbon hydrogen peroxide solution is to add activated carbon into a 30% hydrogen peroxide solution, and stirring at 60 ℃ for 20min to obtain the sodium sulfate purified solution, wherein the mass ratio of the activated carbon to the hydrogen peroxide solution is 4, and the activated carbon is coconut shell activated carbon with the particle size of 0.4-3 mm), stirring at 40 ℃ and 500rpm/min for 40min, and filtering to obtain the sodium sulfate purified solution;
4) And (3) recrystallization: sodium sulfate purified solution at 70 deg.C and vacuum degree of 4 × 10 4 Concentrating under Pa to 3/5 of the original volume, cooling to 40 deg.C, and maintaining for 20min; continuously cooling to 20 ℃ for crystallization for 6h, and washing the obtained crystal with a saturated sodium sulfate solution to obtain a pure sodium sulfate decahydrate product;
5) And (3) drying: drying the pure sodium sulfate decahydrate at 135 ℃ for 14h to obtain anhydrous sodium sulfate.
Example 3
The embodiment provides a method for preparing anhydrous sodium sulphate by viscose acid bath evaporation, which comprises the following steps:
1) Pretreatment: carrying out acid bath aeration treatment on viscose spinning to remove most of sulfide in the viscose spinning, and filtering to remove most of cellulose and solid impurities to obtain acid bath pretreatment liquid;
2) Primary evaporation and crystallization: the acid bath pretreatment solution was heated at 70 ℃ under a vacuum of 4X 10 4 Concentrating under Pa to 1/2 of the original volume; then crystallizing for 3h at 20 ℃, and filtering to obtain a sodium sulfate decahydrate crude product;
3) Redissolving and purifying: adding water into a sodium sulfate decahydrate crude product, dissolving at 50 ℃ to prepare a sodium sulfate redissolution with the mass concentration of 40%, adding a newly prepared activated carbon hydrogen peroxide solution with the volume of 10% of the sodium sulfate redissolution into the sodium sulfate redissolution (wherein the preparation method of the activated carbon hydrogen peroxide solution is to add activated carbon into the hydrogen peroxide solution with the concentration of 40%, stirring at 50 ℃ for 30min to obtain the sodium sulfate purified solution, wherein the mass ratio of the activated carbon to the hydrogen peroxide solution is 4, and the activated carbon is coconut shell activated carbon with the particle size of 0.4-3 mm), stirring at 50 ℃ and 500rpm/min for 40min, and filtering to obtain the sodium sulfate purified solution;
4) And (3) recrystallization: sodium sulfate purified solution at 70 deg.C and vacuum degree of 2 × 10 4 Concentrating under Pa to 3/4 of the original volume, cooling to 45 deg.C, and maintaining for 25min; then cooling to 20 ℃ for crystallization for 4h, and washing the obtained crystal with a saturated sodium sulfate solution to obtain a pure sodium sulfate decahydrate product;
5) And (3) drying: drying the pure sodium sulfate decahydrate at 135 ℃ for 14h to obtain anhydrous sodium sulfate.
Example 4
The embodiment provides a method for preparing anhydrous sodium sulphate by viscose acid bath evaporation, which comprises the following steps:
1) Pretreatment: carrying out acid bath aeration treatment on the viscose for viscose spinning to remove most of sulfide in the viscose, and filtering to remove most of cellulose and solid impurities to obtain acid bath pretreatment liquid;
2) Primary evaporation and crystallization: acid bath pretreatment solution was heated at 65 ℃ under a vacuum of 4X 10 4 Carrying out first reduced pressure evaporation under Pa until the volume is 1/2 of the original volume; then crystallizing for 3h at 18 ℃, and filtering to obtain a sodium sulfate decahydrate crude product;
3) Redissolving and purifying: adding water into a sodium sulfate decahydrate crude product, dissolving at 45 ℃ to prepare a sodium sulfate redissolution with the mass concentration of 40%, adding a newly prepared activated carbon hydrogen peroxide treatment solution with the volume of 13% of the sodium sulfate redissolution into the sodium sulfate redissolution (wherein the preparation method of the activated carbon hydrogen peroxide solution is to add activated carbon into a 30% hydrogen peroxide solution, and stirring at 60 ℃ for 20min to obtain the sodium sulfate purified solution, wherein the mass ratio of the activated carbon to the hydrogen peroxide solution is 4, and the activated carbon is coconut shell activated carbon with the particle size of 0.4-3 mm), stirring at 40 ℃ and 500rpm/min for 40min, and filtering to obtain the sodium sulfate purified solution;
4) And (3) recrystallization: sodium sulfate purified solution at 70 deg.C and vacuum degree of 4 × 10 4 Concentrating under Pa to 3/5 of the original volume, cooling to 40 deg.C, and maintaining for 20min; continuously cooling to 20 ℃ for crystallization for 6h, and washing the obtained crystal with a saturated sodium sulfate solution to obtain a pure sodium sulfate decahydrate product;
5) And (3) drying: drying the pure sodium sulfate decahydrate at 135 ℃ for 14h to obtain anhydrous sodium sulfate.
Comparative example
The difference from example 1 is that the hydrogen peroxide in the activated carbon hydrogen peroxide solution treatment liquid is replaced by equal amount of water, the anhydrous sodium sulphate is prepared by the steps of example 1 in the rest steps, the anhydrous sodium sulphate mass fraction, the water insoluble mass fraction, the zinc mass fraction and the whiteness degree (R457) purity of the anhydrous sodium sulphate prepared in examples 1-4 and comparative example are measured, and the results are shown in Table 1,
TABLE 1 Yuan Min powder Mass determination results
As can be seen from Table 1, the glauber salt prepared in examples 1-4 of the present application has better mass fraction of sodium sulfate and whiteness and lower mass fraction of water-insoluble substances and zinc than the comparative examples, which shows that the hydrogen peroxide solution treating solution using activated carbon in the method of the present invention can better remove water-insoluble substances and zinc in the acid bath of viscose fibers than the activated carbon, so that the glauber salt has higher purity and whiteness and lower impurity content.
Finally, it should be emphasized that the above-described preferred embodiments of the present invention are merely examples of implementations, rather than limitations, and that many variations and modifications of the invention are possible to those skilled in the art, without departing from the spirit and scope of the invention.
Claims (5)
1. A method for preparing anhydrous sodium sulphate by viscose acid bath evaporation is characterized by comprising the following steps:
1) Pretreatment: carrying out aeration and filtration pretreatment on an acid bath for viscose spinning to obtain an acid bath pretreatment solution;
2) Primary evaporation and crystallization: carrying out first reduced pressure evaporation on the acid bath pretreatment liquid, carrying out first cooling crystallization, and filtering to obtain a sodium sulfate decahydrate crude product;
3) Redissolving and purifying: redissolving the crude sodium sulfate decahydrate with water to obtain a sodium sulfate redissolution, adding a newly prepared active carbon hydrogen peroxide treatment solution into the sodium sulfate redissolution, heating, stirring and filtering to obtain a sodium sulfate purified solution; step 3), the active carbon hydrogen peroxide solution treatment liquid accounts for 10-15% of the volume of the sodium sulfate redissolution solution; the preparation method of the active carbon hydrogen peroxide solution in the step 3) is to add the active carbon into the hydrogen peroxide solution and stir the solution for 20 to 30min at the temperature of between 50 and 60 ℃ to obtain the active carbon hydrogen peroxide solution; the concentration of the hydrogen peroxide solution is 30-40%, and the mass ratio of the activated carbon to the hydrogen peroxide solution is (2-4); step 3), the mass concentration of sodium sulfate in the redissolution is 35-40%; the temperature of the redissolution is 40-50 ℃; step 3), the heating and stirring are carried out for 30-40min at the temperature of 40-50 ℃ and the rpm of 300-500;
4) And (3) recrystallization: carrying out secondary reduced pressure evaporation on the sodium sulfate purified solution, carrying out secondary cooling crystallization, and washing crystals with a saturated sodium sulfate solution to obtain a pure sodium sulfate decahydrate product;
5) And (3) drying: and drying the pure sodium sulfate decahydrate to obtain anhydrous sodium sulphate.
2. The method for preparing anhydrous sodium sulphate by acid bath evaporation of viscose fibers as claimed in claim 1, wherein the activated carbon is coconut shell activated carbon with a particle size of 0.4-3 mm.
3. The method for preparing anhydrous sodium sulphate by acid bath evaporation of viscose fibers as claimed in claim 1, wherein the temperature of the first reduced pressure evaporation in step 2) is 60-70 ℃ and the vacuum degree is 2 x 10 4 Pa-8×10 4 Pa；
And/or the first reduced pressure evaporation needs to be concentrated to 1/2-3/4 of the volume of the pretreatment liquid of the acid bath;
and/or the temperature of the first cooling crystallization in the step 2) is 15-20 ℃.
4. The method for preparing anhydrous sodium sulphate by acid bath evaporation of viscose fibers as claimed in claim 1, wherein the temperature of the second reduced pressure evaporation in the step 4) is 60-70 ℃, and the vacuum degree is 2 x 10 4 Pa-8×10 4 Pa；
And/or the second reduced pressure evaporation in the step 4) needs to be concentrated to 3/5-3/4 of the volume of the sodium sulfate purified liquid;
and/or the temperature of the second cooling crystallization in the step 4) is firstly cooled to 40-50 ℃, and is kept for 20-30min; then cooling to 15-20 ℃ for crystallization till crystallization is complete.
5. The method for preparing anhydrous sodium sulphate by acid bath evaporation of viscose fibers as claimed in claim 1, wherein the drying in step 5) is carried out at 120-150 ℃ for 12-14h.
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