CN111636101B - Method for removing metal ions in waste cotton fabric dissolving pulp - Google Patents
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- CN111636101B CN111636101B CN202010329855.4A CN202010329855A CN111636101B CN 111636101 B CN111636101 B CN 111636101B CN 202010329855 A CN202010329855 A CN 202010329855A CN 111636101 B CN111636101 B CN 111636101B
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D1/00—Treatment of filament-forming or like material
- D01D1/02—Preparation of spinning solutions
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
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Abstract
The invention relates to a method for removing metal ions in waste cotton fabric dissolving pulp, which comprises the steps of firstly preparing a removing solution with the pH value of 1-3 by using acid, a complexing agent (a compound of sodium hexametaphosphate and ethylene diamine tetraacetic acid) and deionized water, then mixing the removing solution and the waste cotton fabric dissolving pulp to obtain a mixture, intermittently stirring for a period of time at a certain temperature, and finally centrifuging to remove the solution in the mixture and washing; testing Fe in the treated waste cotton fabric dissolving pulp3+The removal rate of (1) is 80-96%, and Cu2+The removal rate of (1) is 23-56%, and Mn is2+The removal rate of the pulp is 64-92%, and the yield of the pulp is more than or equal to 94%. The method for removing the metal ions in the waste cotton fabric dissolving pulp has a remarkable effect of removing the metal ions in the waste cotton fabric dissolving pulp, is beneficial to subsequent bleaching and spinning, is simple and easy to implement in the whole process, has an excellent effect, and has a great popularization value.
Description
Technical Field
The invention belongs to the technical field of waste textile recovery engineering, and relates to a method for removing metal ions in waste cotton fabric dissolving pulp.
Background
The waste cotton fabric refers to a waste textile with the cotton fiber content of more than 75 percent. In recent years, the production amount of waste cotton fabrics is increasing day by year, and although the utilization modes of the waste cotton fabrics are various, most of the utilization modes have the characteristics of low value, low utilization rate and the like. The waste cotton fabric is made into dissolving pulp through the processes of preimpregnation, cooking, metal ion removal, bleaching and the like, then the dissolving pulp is used as a raw material, and spinning is carried out by utilizing a viscose fiber process or a Lyocell (Lyocell) new solvent method process, so that the method is a high-valued utilization mode capable of being applied on a large scale, the problem that the waste cotton fabric is difficult to utilize or low-valued utilization can be solved, and the dissolving pulp and regenerated cellulose fibers with good performance can be obtained. In the process of preparing dissolving pulp from waste cotton fabrics, the process of removing metal ions is very important, because the metal ions in the waste cotton fabrics are mainly Fe3+、Ca2+、Mn2+、Cu2+、Mg2+And the like, the metal ions can decompose bleaching agents (such as hydrogen peroxide) in the bleaching process, thereby reducing the bleaching efficiency; in addition, if the content of metal ions in the dissolving pulp is too high, N-methylmorpholine-N-oxide (NMMO), which is a solvent used in the lyocell process, is decomposed, and the spinning nozzle is clogged.
In the prior art, the method for removing metal ions mainly utilizes acid treatment and complexing agent treatment. Patent CN201710650004.8 discloses an acid treatment method, which uses hydrochloric acid with a certain concentration to perform acid treatment on pulp for 20-60 min, so as to achieve the effect of removing metal ions, but it will bring the problems of decreasing polymerization degree or yield. Patent CN 200910094561.1 discloses a complexing agent treatment method, mainly by Mg (CH)3COO)2、Ca(CH3COO)2Ethylenediaminetetraacetic acid (EDTA) to complex metal ions, 63% of iron ions can be removed, but Ca is further introduced2+、Mg2+Not only the ash content is increased but also the subsequent spinning is not facilitated. Patent CN201480064674.6 discloses a staged treatment using acid treatment and complexing treatment, or a combined treatment by adding a complexing agent into an acid solution and mixing; the acid treatment is to dissolve and attach on the pulp by using acidThe acid-soluble impurities are removed by centrifugation, the metal ions generally exist in the form of hydroxide, for example, the iron ions exist in the form of ferric hydroxide, after the acid solution is added, the iron ions are changed into the iron ions from the ferric hydroxide, at the moment, the free iron ions can be removed by water washing, and because the solubility product constant of the iron ions is unstable, the free iron ions can be changed into the iron hydroxide to be attached to the fibers due to the increase of the pH value in the process of removing the iron ions, so that the removal rate of the metal ions is not high, and the lower the pH value of the acid is, the better the effect of removing the metal ions is, but the lower the pH value is, the more serious the degradation of the fibers is, so that the yield and the polymerization degree of the pulp are reduced; in the complexing agent treatment, the complexing agent can be used for directly complexing metal ions, but the metal ions exist in the form of hydroxide, the solubility product of the metal ions is low, the complexing agent cannot easily capture the metal ions to form a chelate so as to be washed out, the rate of complexing the metal ions by the complexing agent is low, and the removal rate of the metal ions is also low; the complexing agent is added into acid for combination treatment, although the metal compound can be changed into free metal ions to be beneficial to complexing, the complexing agent is not in an optimal complexing structure at the pH value possibly, and the complexing effect is reduced.
Therefore, the research on a method for efficiently removing metal ions to realize efficient bleaching while protecting cellulose from being excessively degraded when preparing the waste cotton fabric dissolving pulp has very important significance.
Disclosure of Invention
The invention aims to solve the problems of low metal ion removal rate and cellulose degradation in the process of preparing waste cotton fabric dissolving pulp in the prior art, and provides a method for removing metal ions in the waste cotton fabric dissolving pulp.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a method for removing metal ions in waste cotton fabric dissolving pulp adopts a solution with a pH value of 1-3 and containing a complexing agent and an acid, wherein the complexing agent is a compound of sodium hexametaphosphate and ethylene diamine tetraacetic acid.
The complex of sodium hexametaphosphate and ethylenediamine tetraacetic acid is used as the complexing agent, so that the removal rate of metal ions is effectively improved, and cellulose degradation is avoided. The complexing agent (the compound of sodium hexametaphosphate and ethylene diamine tetraacetic acid) still has good complexing ability when the pH value is 1-3, and both acid and metal ions can fully play roles. The acid is beneficial to changing the metal ions from the binding state to the free state, the complexing agent can complex the free metal ions, the advantages of the acid and the complexing agent are complementary, and the effect is good. The invention uses ethylene diamine tetraacetic acid as a main complexing agent and sodium hexametaphosphate as an auxiliary complexing agent, the structures of the ethylene diamine tetraacetic acid and the sodium hexametaphosphate contain coordination groups such as amino, carboxyl and the like, the groups contain coordination atoms, the coordination atoms and metal ions such as iron ions form coordination bonds to further chelate into compounds, the metal chelate compounds can leave the cotton fiber with the cleaning liquid after being washed, the complexing effect of the ethylene diamine tetraacetic acid is stronger, so that the main complexing agent, the ethylene diamine tetraacetic acid, has poor dispersibility and solubility in water solution at normal temperature, the sodium hexametaphosphate has the characteristics of a surfactant, can help the ethylenediamine tetraacetic acid to be fully dispersed in the treatment liquid and promote the dissolution, and the contact probability of the ethylenediamine tetraacetic acid and the metal ions in the waste cotton fabric dissolving pulp is further improved, so that the dissociated metal ions and the uniformly dispersed complexing agent can be in full contact, and the metal ions in the waste cotton fabric dissolving pulp can be efficiently removed. In addition, the complexing effect of the ethylene diamine tetraacetic acid on metal ions such as iron ions, copper ions, manganese ions and the like is good, the removing effect of the sodium hexametaphosphate on calcium ions and magnesium ions is good, and the metal ions in the pulp can be effectively removed by the composite complexing of the ethylene diamine tetraacetic acid and the sodium hexametaphosphate, so that the quality of the pulp is improved.
As a preferred technical scheme:
according to the method for removing metal ions in the waste cotton fabric dissolving pulp, the molar ratio of sodium hexametaphosphate to ethylene diamine tetraacetic acid is 1: 1-3, the sodium hexametaphosphate is used as an auxiliary complexing agent, so that the addition amount of the sodium hexametaphosphate is less than that of the ethylene diamine tetraacetic acid, and the sodium hexametaphosphate can play a role in dispersing the ethylene diamine tetraacetic acid, so that the addition amount is not too low, otherwise the dispersing effect is influenced, the addition amount is not too high, otherwise the cost is increased, and pollution is caused.
The method for removing the metal ions in the waste cotton fabric dissolving pulp comprises the following specific steps: firstly, preparing a removing solution from acid, a complexing agent and deionized water, then mixing the removing solution with waste cotton fabric dissolving pulp to obtain a mixture, intermittently stirring for a period of time at a certain temperature, finally centrifuging to remove the solution in the mixture, and washing. The invention separates metal ions by adopting a centrifugal and deionized water washing mode, so that the metal ions can be largely separated from the waste cotton fabric dissolving pulp, and the aim of removing the metal ions is fulfilled.
According to the method for removing the metal ions in the waste cotton fabric dissolving pulp, the mass ratio of the acid to the complexing agent in the removing liquid is 7-20: 1, and the acid is inorganic acid (such as dilute sulfuric acid); the addition amount of the acid has a large influence on the removal rate of the metal ions of the dissolving pulp, and when the addition amount of the acid is high, the dissolution of the metal hydroxide precipitate is increased, so that the removal rate of the metal ions is improved, but the yield of the pulp is also reduced; when the acid addition amount is less, the pulp yield is reduced less, but the dissolving effect of the metal hydroxide precipitate is insufficient, the complexing agent is difficult to fully complex the metal ions, and the removal rate of the metal ions is reduced.
According to the method for removing the metal ions in the waste cotton fabric dissolving pulp, the solid content of the waste cotton fabric dissolving pulp is 20-50% (the solid content of the dissolving pulp after centrifugal treatment is generally in the range), the cotton fiber content of the waste cotton fabric is more than 70 wt%, and the mass addition amount of the complexing agent is 0.05-0.8% of the absolute dry mass of the waste cotton fabric dissolving pulp.
The method for removing the metal ions in the waste cotton fabric dissolving pulp has the advantages that the certain temperature is 30-90 ℃, and the intermittent stirring is carried out, namely, the stirring is carried out once every 3-10 min, and the period of time is 30-90 min.
According to the method for removing the metal ions in the waste cotton fabric dissolving pulp, deionized water is used for washing, the washing frequency is 2-6 times, and the washing termination condition is that the pH value of the water washing liquid reaches 7.0-7.5. Washing is a process of washing acidic dissolving pulp to be neutral, and when the pH value is in the range, the dissolving pulp is washed.
The method for removing metal ions in the waste cotton fabric dissolving pulp is Fe in the waste cotton fabric dissolving pulp3+The removal rate of (1) is 80-96%, and Cu2+The removal rate of (1) is 23-56%, and Mn is2+The removal rate of the pulp is 64-92%, and the yield of the pulp is more than or equal to 94%. Note: the pulp of the invention is cotton pulp, Fe3+The content of (A) is determined by the method described in textile industry Standard FZ/T50010.6-1998 (determination of the iron content of pulp for viscose fibers), Cu2+The content of (B) is measured by the method described in the national Standard GB/T8941.3-2008 (measurement of copper content in paper, paperboard and pulp), Mn2+The content of (A) is measured by the method described in the national standard GB/T8943.3-2008 (measurement of manganese content of paper, paperboard and pulp).
Has the advantages that:
(1) according to the method for removing the metal ions in the waste cotton fabric dissolving pulp, the effect of removing the metal ions in the waste cotton fabric dissolving pulp is obvious, the pulp yield is high, and the subsequent bleaching and spinning are facilitated;
(2) the method for removing the metal ions in the waste cotton fabric dissolving pulp is simple and easy to implement, low in cost and extremely high in popularization value.
Detailed Description
The invention will be further illustrated with reference to specific embodiments. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
Example 1
A method for removing metal ions in waste cotton fabric dissolving pulp comprises the following specific steps:
(1) preparing inorganic acid (65 wt% dilute sulfuric acid), complexing agent (a compound of sodium hexametaphosphate and ethylene diamine tetraacetic acid with a molar ratio of 1: 1) and deionized water into a removing solution with a pH value of 1, wherein the mass ratio of the inorganic acid to the complexing agent is 10: 1;
(2) mixing the removing solution with waste cotton fabric dissolving pulp with solid content of 30% to obtain a mixture, and stirring once every 9min at 40 ℃ for 70 min; wherein the cotton fiber content of the waste cotton fabrics is 71 wt%, and the mass addition amount of the complexing agent is 0.8% of the absolute dry mass of the waste cotton fabric dissolving pulp;
(3) centrifuging to remove the solution in the mixture, and washing with deionized water for 3 times, wherein the washing termination condition is that the pH value of the water washing solution reaches 7.1;
by the method, Fe in the waste cotton fabric dissolving pulp3+Has a removal rate of 96% (determined according to the method of FZ/T50010.6-1998), Cu2+Has a removal rate of 56% (measured according to the method of GB/T8943.1-2008), Mn2 +The removal rate of (2) was 92% (measured by the method of GB/T8943.3-2008), and the yield of pulp was 95%.
Comparative example 1
The specific process of the method for removing metal ions in the waste cotton fabric dissolving pulp is basically the same as that in the example 1, the difference is only that sodium hexametaphosphate in the complexing agent is replaced by diethylenetriamine pentahydroxy acid salt, and Fe in the waste cotton fabric dissolving pulp3+The removal rate of (D) was 83% (measured by the method of FZ/T50010.6-1998), and the yield of pulp was 86%.
As can be seen by comparing comparative example 1 with example 1, Fe in comparative example 13+The removal rate is lower, the pulp yield is lower, because sodium hexametaphosphate in example 1 is an auxiliary complexing agent and plays a role in dispersing the ethylenediamine tetraacetic acid, but diethylenetriamine pentahydroxy acid salt is added in comparative example 1, and only plays a role in complexing, but does not play a role in dispersing the ethylenediamine tetraacetic acid, so that the dispersing effect of the ethylenediamine tetraacetic acid is obviously poorer than that of example 1, and the complexing effect of the ethylenediamine tetraacetic acid is reduced.
Comparative example 2
The specific process of the method for removing the metal ions in the waste cotton fabric dissolving pulp is basically the same as that in the embodiment 1, the difference is that the complexing agent does not contain sodium hexametaphosphate, and the waste cotton fabric dissolving pulp contains Fe3+The removal rate of (D) was 80%, and the yield of pulp was87％。
As can be seen by comparing comparative example 2 with example 1, Fe in comparative example 23+The removal rate is lower, the pulp yield is lower, because the comparative example 2 does not contain sodium hexametaphosphate, can not assist the complexation, also causes the dispersing effect of the ethylene diamine tetraacetic acid to be obviously worse than that of the example 1, and reduces the complexation effect of the ethylene diamine tetraacetic acid.
Comparative example 3
The specific process of the method for removing the metal ions in the waste cotton fabric dissolving pulp is basically the same as that in the embodiment 1, the difference is only that the mass ratio of the inorganic acid to the complexing agent is 30:1, and the Fe in the waste cotton fabric dissolving pulp3+The removal rate of (2) was 85% (measured by the method of FZ/T50010.6-1998), and the yield of pulp was 76%.
As can be seen by comparing comparative example 3 with example 1, Fe in comparative example 33+The removal rate was lower and the pulp yield was lower because the acid addition amount in comparative example 3 was larger, which, although increasing the dissolution of the metal compound, adversely affected the metal ion complexation and decreased the pulp yield.
Example 2
A method for removing metal ions in waste cotton fabric dissolving pulp comprises the following specific steps:
(1) preparing inorganic acid (dilute sulfuric acid with the concentration of 70 wt%), complexing agent (compound of sodium hexametaphosphate and ethylene diamine tetraacetic acid with the molar ratio of 1: 2) and deionized water into a removing solution with the pH value of 2, wherein the mass ratio of the inorganic acid to the complexing agent is 15: 1;
(2) mixing the removing solution with waste cotton fabric dissolving pulp with solid content of 25% to obtain a mixture, and stirring once at intervals of 8min at 50 ℃ for 80 min; wherein the cotton fiber content of the waste cotton fabrics is 72 wt%, and the mass addition amount of the complexing agent is 0.3% of the absolute dry mass of the waste cotton fabric dissolving pulp;
(3) centrifuging to remove the solution in the mixture, and washing for 2 times by using deionized water, wherein the washing termination condition is that the pH value of the water washing liquid reaches 7.0;
by the method, Fe in the waste cotton fabric dissolving pulp3+Removal ofThe ratio was 92% (determined by the method of FZ/T50010.6-1998), Cu2+Has a removal rate of 49% (measured according to the method of GB/T8943.1-2008), and Mn2 +The removal rate of (D) was 82% (measured by the method of GB/T8943.3-2008), and the yield of pulp was 97%.
Example 3
A method for removing metal ions in waste cotton fabric dissolving pulp comprises the following specific steps:
(1) preparing inorganic acid (65 wt% dilute sulfuric acid), complexing agent (a compound of sodium hexametaphosphate and ethylene diamine tetraacetic acid with a molar ratio of 1: 3) and deionized water into a removing solution with a pH value of 2, wherein the mass ratio of the inorganic acid to the complexing agent is 7: 1;
(2) mixing the removing solution with waste cotton fabric dissolving pulp with solid content of 35% to obtain a mixture, stirring once every 10min at 30 ℃, and stirring for 90 min; wherein the cotton fiber content of the waste cotton fabrics is 71 wt%, and the mass addition amount of the complexing agent is 0.5% of the absolute dry mass of the waste cotton fabric dissolving pulp;
(3) centrifuging to remove the solution in the mixture, and washing with deionized water for 3 times, wherein the washing termination condition is that the pH value of the water washing solution reaches 7.2;
by the method, Fe in the waste cotton fabric dissolving pulp3+The removal rate of (A) was 91% (determined by the method of FZ/T50010.6-1998), Cu2+Has a removal rate of 52% (measured according to the method of GB/T8943.1-2008), Mn2 +The removal rate of (D) was 85% (measured by the method of GB/T8943.3-2008), and the yield of pulp was 98%.
Example 4
A method for removing metal ions in waste cotton fabric dissolving pulp comprises the following specific steps:
(1) preparing inorganic acid (dilute sulfuric acid with the concentration of 66 wt%), complexing agent (compound of sodium hexametaphosphate and ethylene diamine tetraacetic acid with the molar ratio of 1: 2) and deionized water into a removing solution with the pH value of 3, wherein the mass ratio of the inorganic acid to the complexing agent is 8: 1;
(2) mixing the removing solution with waste cotton fabric dissolving pulp with solid content of 20% to obtain a mixture, and stirring once every 5min at 60 ℃ for 60 min; wherein the cotton fiber content of the waste cotton fabrics is 75 wt%, and the mass addition amount of the complexing agent is 0.4% of the absolute dry mass of the waste cotton fabric dissolving pulp;
(3) centrifuging to remove the solution in the mixture, and washing for 2 times by using deionized water, wherein the washing termination condition is that the pH value of the water washing liquid reaches 7.3;
by the method, Fe in the waste cotton fabric dissolving pulp3+Has a removal rate of 85% (determined according to the method of FZ/T50010.6-1998), Cu2+Has a removal rate of 43% (measured according to the method of GB/T8943.1-2008), Mn2 +The removal rate of (D) was 79% (measured by the method of GB/T8943.3-2008), and the yield of pulp was 99%.
Example 5
A method for removing metal ions in waste cotton fabric dissolving pulp comprises the following specific steps:
(1) preparing inorganic acid (dilute sulfuric acid with the concentration of 60 wt%), complexing agent (compound of sodium hexametaphosphate and ethylene diamine tetraacetic acid with the molar ratio of 1: 2) and deionized water into a removing solution with the pH value of 2, wherein the mass ratio of the inorganic acid to the complexing agent is 15: 1;
(2) mixing the removing solution with waste cotton fabric dissolving pulp with solid content of 35% to obtain a mixture, and stirring once at intervals of 7min at 55 ℃ for 50 min; wherein the cotton fiber content of the waste cotton fabrics is 73 wt%, and the mass addition amount of the complexing agent is 0.2% of the absolute dry mass of the waste cotton fabric dissolving pulp;
(3) centrifuging to remove the solution in the mixture, and washing with deionized water for 4 times, wherein the washing termination condition is that the pH value of the water washing solution reaches 7.3;
by the method, Fe in the waste cotton fabric dissolving pulp3+The removal rate of (A) was 91% (determined by the method of FZ/T50010.6-1998), Cu2+Has a removal rate of 48% (measured according to the method of GB/T8943.1-2008), Mn2 +The removal rate of (D) was 80% (measured by the method of GB/T8943.3-2008), and the yield of pulp was 98%.
Example 6
A method for removing metal ions in waste cotton fabric dissolving pulp comprises the following specific steps:
(1) preparing inorganic acid (dilute sulfuric acid with the concentration of 68 wt%), complexing agent (compound of sodium hexametaphosphate and ethylene diamine tetraacetic acid with the molar ratio of 1: 2) and deionized water into a removing solution with the pH value of 2, wherein the mass ratio of the inorganic acid to the complexing agent is 17: 1;
(2) mixing the removing solution with waste cotton fabric dissolving pulp with solid content of 40% to obtain a mixture, and stirring once at intervals of 4min at 70 ℃ for 40 min; wherein the cotton fiber content of the waste cotton fabrics is 72 wt%, and the mass addition amount of the complexing agent is 0.1% of the absolute dry mass of the waste cotton fabric dissolving pulp;
(3) centrifuging to remove the solution in the mixture, and washing with deionized water for 5 times, wherein the washing termination condition is that the pH value of the water washing solution reaches 7.2;
by the method, Fe in the waste cotton fabric dissolving pulp3+Has a removal rate of 93% (determined according to the method of FZ/T50010.6-1998), Cu2+Has a removal rate of 44% (measured according to the method of GB/T8943.1-2008), and Mn2 +The removal rate of (2) was 76% (measured by the method of GB/T8943.3-2008), and the yield of pulp was 96%.
Example 7
A method for removing metal ions in waste cotton fabric dissolving pulp comprises the following specific steps:
(1) preparing inorganic acid (65 wt% dilute sulfuric acid), complexing agent (compound of sodium hexametaphosphate and ethylene diamine tetraacetic acid with the molar ratio of 1: 2) and deionized water into a removing solution with the pH value of 3, wherein the mass ratio of the inorganic acid to the complexing agent is 20: 1;
(2) mixing the removing solution with waste cotton fabric dissolving pulp with solid content of 45% to obtain a mixture, and stirring once at intervals of 4min at 75 ℃ for 45 min; wherein the cotton fiber content of the waste cotton fabrics is 71 wt%, and the mass addition amount of the complexing agent is 0.05% of the absolute dry mass of the waste cotton fabric dissolving pulp;
(3) centrifuging to remove the solution in the mixture, and washing with deionized water for 5 times, wherein the washing termination condition is that the pH value of the water washing solution reaches 7.4;
by the method, Fe in the waste cotton fabric dissolving pulp3+Has a removal rate of 80% (determined according to the method of FZ/T50010.6-1998), Cu2+Has a removal rate of 39% (measured according to the method of GB/T8943.1-2008), and Mn2 +The removal rate of (2) was 74% (measured by the method of GB/T8943.3-2008), and the yield of pulp was 99%.
Example 8
A method for removing metal ions in waste cotton fabric dissolving pulp comprises the following specific steps:
(1) preparing inorganic acid (dilute sulfuric acid with the concentration of 60 wt%), complexing agent (compound of sodium hexametaphosphate and ethylene diamine tetraacetic acid with the molar ratio of 1: 3) and deionized water into a removing solution with the pH value of 3, wherein the mass ratio of the inorganic acid to the complexing agent is 9: 1;
(2) mixing the removing solution with waste cotton fabric dissolving pulp with solid content of 50% to obtain a mixture, and stirring once at 80 ℃ every 3min for 30 min; wherein the cotton fiber content of the waste cotton fabrics is 74 wt%, and the mass addition amount of the complexing agent is 0.3% of the absolute dry mass of the waste cotton fabric dissolving pulp;
(3) centrifuging to remove the solution in the mixture, and washing with deionized water for 6 times, wherein the washing termination condition is that the pH value of the water washing solution reaches 7.5;
by the method, Fe in the waste cotton fabric dissolving pulp3+Has a removal rate of 80% (determined according to the method of FZ/T50010.6-1998), Cu2+Has a removal rate of 23% (measured according to the method of GB/T8943.1-2008), Mn2 +The removal rate of (2) was 64% (measured by the method of GB/T8943.3-2008), and the yield of pulp was 94%.
Claims (5)
1. A method for removing metal ions in waste cotton fabric dissolving pulp is characterized by comprising the following steps: firstly, preparing acid, a complexing agent and deionized water into a removing solution with the pH value of 1-3, then mixing the removing solution with waste cotton fabric dissolving pulp to obtain a mixture, intermittently stirring for a period of time at a certain temperature, and finally centrifuging to remove the solution in the mixture and washing; the washing termination condition is that the pH value of the washing liquid reaches 7.0-7.5; the complexing agent is a compound of sodium hexametaphosphate and ethylene diamine tetraacetic acid in a molar ratio of 1: 1-3; acid(s)Is inorganic acid; fe in waste cotton fabric dissolving pulp3+The removal rate of (1) is 80-96%, and Cu2+The removal rate of (1) is 23-56%, and Mn is2+The removal rate of the pulp is 64-92%, and the yield of the pulp is more than or equal to 94%.
2. The method for removing metal ions in waste cotton fabric dissolving pulp according to claim 1, wherein the mass ratio of acid to complexing agent in the removing solution is 7-20: 1.
3. The method for removing metal ions from the waste cotton fabric dissolving pulp according to claim 1, wherein the solid content of the waste cotton fabric dissolving pulp is 20-50%, the cotton fiber content of the waste cotton fabric is more than 70 wt%, and the mass addition amount of the complexing agent is 0.05-0.8% of the absolute dry mass of the waste cotton fabric dissolving pulp.
4. The method for removing metal ions from waste cotton fabric dissolving pulp according to claim 1, wherein the certain temperature is 30-90 ℃, and the intermittent stirring is performed once every 3-10 min for 30-90 min.
5. The method for removing metal ions in waste cotton fabric dissolving pulp according to claim 1, wherein deionized water is adopted for washing, and the washing times are 2-6 times.
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| CN114150521B (en) * | 2021-12-03 | 2023-02-10 | 太原理工大学 | Preparation method of hemp-based lyocell fiber pulp |
| CN115125751A (en) * | 2022-06-01 | 2022-09-30 | 齐鲁工业大学 | Method for cleanly and efficiently preparing cotton pulp from waste cotton textiles |
| CN114984917A (en) * | 2022-06-01 | 2022-09-02 | 齐鲁工业大学 | Method for efficiently removing metal ions in waste cotton fabric regeneration pulp |
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