CN115873151A - Preparation method of brominated polymer - Google Patents
Preparation method of brominated polymer Download PDFInfo
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- CN115873151A CN115873151A CN202111130947.0A CN202111130947A CN115873151A CN 115873151 A CN115873151 A CN 115873151A CN 202111130947 A CN202111130947 A CN 202111130947A CN 115873151 A CN115873151 A CN 115873151A
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Abstract
The invention discloses a preparation method of a brominated polymer, which comprises the following steps: 1) Contacting the polymer solution with liquid bromine to obtain a brominated polymer solution; 2) Contacting the brominated polymer solution with hot water and water vapor, and separating to obtain brominated colloidal particle water and an organic solvent; 3) Dehydrating the brominated colloidal particle water obtained in the step 2) to obtain brominated polymer and bromine-containing wastewater; 4) Contacting at least one part of the bromine-containing wastewater obtained in the step 3) with an organic extractant to obtain bromine-containing wastewater without rubber powder; 5) The bromine-containing waste water without the rubber powder is used as process water and/or bromine is recovered; 6) The residual part of the bromine-containing wastewater obtained in the step 3) is reused as hot water in the step 2). The wastewater without the rubber powder obtained by the method can be used for recovering bromine or used as process water such as washing water and the like; the process operation of brominated polymer and bromine recovery is stabilized, and the loss of brominated polymer and the discharge amount of wastewater are reduced.
Description
Technical Field
The invention belongs to the technical field of polymer preparation, and particularly relates to a preparation method of a brominated polymer.
Background
The polymer can be modified or added with the performance of the polymer through bromination, and the application field of the polymer is widened. For example, bromobutyl rubber obtained by bromination of butyl rubber overcomes the defects of poor adhesion, slow vulcanization speed, difficulty in blending with other rubbers and the like, and becomes a preferred material for preparing an inner liner of a tire. The butyl rubber alkane solution is industrially contacted with liquid bromine, and the bromobutyl rubber is prepared by bromine substitution reaction, wherein the theoretical utilization rate of bromine atoms is 50 percent, and the rest 50 percent is converted into hydrogen bromide. And the actual industrial utilization rate is less than 50%, more than half of bromine enters the wastewater in the form of bromide ions, and the content of the bromide ions in the wastewater is higher. If the waste water is directly discharged, the environment is seriously polluted and resources are wasted, so that the method has remarkable social and economic benefits for treating the waste water containing the bromide ions.
The industrial method for recovering bromine from bromine-containing wastewater includes extraction method and distillation method. The distillation method refers to a relatively mature seawater oxidation bromine blowing technology: the bromobutyl rubber waste water is preheated, oxidized by chlorine and distilled by steam to obtain crude bromine, and then is rectified to obtain liquid bromine with 98 percent content, and the recovered liquid bromine can be used as the raw material for producing the bromobutyl rubber again. However, bromine-containing wastewater is derived from separation of glue solution and water, the glue solution and the water phase are difficult to separate due to calcium stearate, antioxidant and other substances contained in the glue solution with the concentration of 15-40wt%, the obtained bromine-containing wastewater contains polymer macromolecular substances which are industrially called as glue powder, although the content of the glue powder in the wastewater is not high, the polymer macromolecular substances are easy to aggregate and bond, the device is blocked, the wastewater has to be stopped periodically, and the operation cost is increased. Meanwhile, the existence of the rubber powder influences the application of bromine-containing wastewater as washing water and process water, and increases the discharge amount of the wastewater.
Disclosure of Invention
In order to improve the technical problem, the invention provides a preparation method of brominated polymer, which comprises the following steps:
1) Contacting the polymer solution with liquid bromine to obtain a brominated polymer solution;
2) Contacting the brominated polymer solution with hot water and water vapor, and separating to obtain brominated colloidal particle water and an organic solvent;
3) Dehydrating the brominated colloidal particle water obtained in the step 2) to obtain brominated polymer and bromine-containing wastewater;
4) Contacting at least one part of the bromine-containing wastewater obtained in the step 3) with an organic extractant to obtain bromine-containing wastewater without rubber powder;
5) The bromine-containing waste water without the crumb rubber is used as process water and/or for recovering bromine;
6) The residual part of the bromine-containing wastewater obtained in the step 3) is reused as hot water in the step 2).
According to the invention, the method comprises the following steps:
1) Contacting the polymer solution with liquid bromine to obtain a brominated polymer solution;
2') carrying out contact washing on the brominated polymer solution obtained in the step 1) and washing water, carrying out phase separation, obtaining a brominated polymer solution phase at the top and obtaining a bromide ion-containing water phase at the bottom;
contacting the brominated polymer solution phase with hot water and water vapor, and separating to obtain brominated colloidal particle water and an organic solvent;
3) Dehydrating the brominated colloidal particle water in the step 2') to obtain brominated polymer and bromine-containing wastewater;
4) Contacting at least a part of the bromine-containing wastewater obtained in the step 3) with an organic extractant to obtain bromine-containing wastewater without rubber powder;
5) The bromine-containing waste water without the crumb rubber is used as process water and/or for recovering bromine;
6) The remaining portion of the bromine-containing waste water obtained in step 3) is recycled as hot water in step 2 ') and/or as washing water in step 2').
According to the invention, the method further comprises the steps of:
7) Contacting the water phase containing bromide ions in the step 2') with an organic extractant to obtain the waste water containing bromide ions without rubber powder;
8) The bromine ion-containing wastewater without the rubber powder in the step 7) is used for recovering bromine.
According to the present invention, in the step 1), the polymer may be at least one of butyl rubber, polybutadiene, styrene-butadiene copolymer; the brominated polymer is one or a mixture of brominated butyl rubber, brominated polybutadiene and brominated styrene-butadiene copolymer.
According to the invention, in step 1), the polymer solution is obtained by dissolving a polymer in an organic solvent.
According to the present invention, the organic solvent in the polymer solution of step 1) includes, but is not limited to, C4-C8 alkanes; for example, it may be at least one of n-pentane, cyclopentane, hexane (which may be, for example, n-hexane, 2-methylpentane, 3-methylpentane, 2,3-dimethylbutane or 2,2-dimethylbutane), cyclohexane, or n-heptane, or a mixture thereof.
According to the invention, in step 2), before the brominated polymer solution is contacted with hot water and steam, alkali and/or a reducing agent can be added into the brominated polymer solution. For example, the brominated polymer solution may be contacted, reacted with a base and/or a reducing agent, and then contacted with hot water and steam. For example, when the alkali and the reducing agent are added simultaneously, the reducing agent is added first, and then the alkali is added so that the pH of the system is 5 to 13, preferably 8 to 9.
According to the present invention, in step 2'), a base and/or a reducing agent may be further added to the brominated polymer solution phase before the brominated polymer solution phase is contacted with hot water and steam. For example, the brominated polymer solution phase may be contacted, reacted with a base and/or a reducing agent, and then contacted with hot water and water vapor. For example, when the alkali and the reducing agent are added simultaneously, the reducing agent is added first, and then the alkali is added so that the pH of the system is 5 to 13, preferably 8 to 9.
The base is illustratively an alkali metal or alkaline earth metal hydroxide, an alkali metal carbonate, an alkali metal bicarbonate, and may be, for example, at least one of sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate, sodium bicarbonate, potassium bicarbonate, or the like; the reducing agent is used for reducing unreacted bromine in the brominated polymer solution and is alkali metal sulfite or pyrosulfite, such as sodium sulfite or sodium pyrosulfite.
Illustratively, the mass of the reducing agent is 0 to 0.1wt% of the mass of the bromobutyl rubber solution.
According to the invention, in step 2) and step 2'), the temperature of the hot water is 50 to 100 ℃, exemplary 50 ℃, 55 ℃, 60 ℃, 65 ℃,70 ℃, 75 ℃, 80 ℃, 85 ℃, 90 ℃, 95 ℃ or 100 ℃; the pressure of the water vapor is 0.2 to 4MPa, and is exemplified by 0.2MPa, 0.5MPa, 0.8MPa, 1.0MPa, 1.5MPa, 1.8MPa, 2MPa, 2.5MPa, 3MPa, 3.5MPa or 4MPa.
According to the invention, step 2') comprises: and (3) carrying out contact washing on the brominated polymer solution and washing water in a container, carrying out phase separation, obtaining a brominated polymer solution phase at the top and obtaining a bromide ion-containing water phase at the bottom. Wherein the brominated polymer solution phase is used in contact with hot water and water vapor.
Illustratively, the vessel in which the brominated polymer solution is contacted with wash water (e.g., process water) for washing includes a column, a tank, and the like.
According to the invention, step 2') is specifically that the bromopolymer solution and washing water are contacted and washed in a washing tower, a bromopolymer solution phase is obtained at the tower top, and a bromide ion-containing water phase is obtained at the tower bottom; and sequentially adding a reducing agent and alkali into the brominated polymer solution phase to ensure that the pH of the system is 5-13, contacting the neutralized brominated polymer solution phase with hot water and water vapor, and separating to obtain brominated colloidal particle water and an organic solvent.
Illustratively, the mass ratio of the brominated polymer solution to the washing water (e.g., process water) is (1-6): 1, and for example, it can be 1:1, 1.2, 1.3, 1.5.
Illustratively, the wash water is one of process water, lye, an aqueous solution containing a reducing agent, bromine-containing wastewater, or bromine-containing wastewater without fines.
Illustratively, the lye is an aqueous solution of a base, the base and the reducing agent having the meaning defined hereinabove.
According to the invention, in the step 2), the container for contacting the brominated polymer solution with hot water and water vapor comprises a tower, a kettle, a tank and the like.
According to the invention, in step 2'), the container for contacting the brominated polymer solution phase with hot water and water vapor comprises a tower, a kettle, a tank and the like.
According to the invention, the content of the rubber powder in the bromine-containing wastewater in the step 3) is not higher than 0.35wt%.
According to the invention, the glue powder comprises a brominated polymer.
According to the invention, the bromine-containing waste water in step 3) can also be reused as washing water for contacting with the brominated polymer solution in step 2').
According to the invention, in the step 4), the mass ratio of the bromine-containing wastewater to the organic extractant is 1 (0.1-1); the contact temperature is 20-100 ℃. For example, it may be 20 ℃, 30 ℃, 40 ℃, 50 ℃, 60 ℃,70 ℃, 80 ℃, 90 ℃ or 100 ℃.
According to the invention, in step 4), the mass of the bromine-containing waste water contacted with the organic extractant is 1 to 30wt%, illustratively 2,3, 5, 7, 10, 12.5, 15, 20, 25 or 30% of the total mass of the bromine-containing waste water.
Illustratively, the bromine-containing wastewater and the organic extractant are contacted in a vessel, and specifically, the contacting vessel comprises a tower, a kettle, a tank and the like.
According to the invention, in the step 7), the mass ratio of the bromide ion-containing aqueous phase to the organic extractant is 1 (0.1-1); the contact temperature is 20-100 ℃. For example, it may be 20 ℃, 30 ℃, 40 ℃, 50 ℃, 60 ℃,70 ℃, 80 ℃, 90 ℃ or 100 ℃.
According to the invention, in step 7), the bromide ion-containing aqueous phase is entirely contacted with the organic extractant. Illustratively, the aqueous phase containing bromide ions and the organic extractant are contacted in a vessel, specifically, the vessel comprises a column, a tank, or the like.
According to the invention, the organic extractant is an organic solvent in which the brominated polymer is dissolved, and the organic extractant contains 0-5wt% of the brominated polymer.
According to the present invention, as described in step 5), the bromine-containing waste water without the crumb rubber obtained in step 4) may be used as process water in the production of the brominated polymer or may be introduced into a debromination recovery unit for recovering bromine, and the process water includes washing water for the brominated polymer solution (for example, the water for washing the brominated polymer solution and water in contact therewith in step 1 may be the waste water without the crumb rubber), lye preparation water (for example, the above-mentioned alkali to be added is added in the form of a lye, and the water for preparing the lye may be the waste water without the crumb rubber), reducing agent solution preparation water (for example, the above-mentioned reducing agent to be added is added in the form of a reducing agent solution, and the water for preparing the reducing agent solution may be the waste water without the crumb rubber), machine seal water for a pump, equipment washing water, and the like.
According to the invention, the bromine ion-containing wastewater obtained in step 7) and free of gum dust is used for bromine recovery as described in step 8).
According to the invention, in step 6), the remaining part of the bromine-containing waste water is divided into two parts, 0 to 30% by weight being used as washing water in step 2 ') and 70 to 100% being reused as hot water in step 2').
According to the invention, in step 6), the mass of the remaining portion of the bromine-containing wastewater is 70 to 97wt%, such as 70 to 95wt%, further such as 80 to 90wt%, exemplarily 70, 75, 76, 77, 78, 79, 80, 85 or 90wt% of the total mass of the bromine-containing wastewater.
The invention has the beneficial effects that:
the invention extracts and phase-separates bromine-containing waste water or bromine ion-containing water phase in the preparation process of brominated polymer by organic solvent to obtain waste water without rubber powder, the waste water without rubber powder can enter a bromine recovery unit for recovering bromine, or be used as process water for preparing auxiliary agents (such as alkali, reducing agent, etc.); the process operation of brominated polymer and bromine recovery is stabilized, and the loss of brominated polymer and the discharge amount of wastewater are reduced.
Detailed Description
The technical solution of the present invention will be further described in detail with reference to specific embodiments. It is to be understood that the following examples are only illustrative and explanatory of the present invention and should not be construed as limiting the scope of the present invention. All the technologies realized based on the above-mentioned contents of the present invention are covered in the protection scope of the present invention.
Unless otherwise indicated, the raw materials and reagents used in the following examples are all commercially available products or can be prepared by known methods.
Example 1
1) And (3) contacting bromine with a butyl rubber hexane solution to perform substitution reaction to obtain a hexane solution containing bromobutyl rubber and hydrogen bromide, namely the bromobutyl rubber reaction solution.
2) Adding 40kg/h 10% sodium sulfite aqueous solution into obtained bromobutyl rubber reaction liquid 6700kg/h (containing bromobutyl rubber 1020 kg/h), then neutralizing with sodium hydroxide solution until pH =9, putting the bromobutyl rubber glue solution after neutralization into a water precipitation and condensation unit, contacting with 2MPa water vapor and 75 ℃ hot water, and separating to obtain hexane solvent and brominated rubber particle water.
3) Dehydrating the brominated colloidal particles in the step 2) to obtain the bromobutyl rubber and bromine-containing wastewater with the flow of about 16t/h and the temperature of 80 ℃.
4) Contacting 2t/h of bromine-containing wastewater (with the content of the rubber powder being 0.35 wt%) with 1t/h of hexane in an extraction tower, removing the rubber powder in the bromine-containing wastewater, and carrying out phase separation to obtain 2t/h of wastewater without the rubber powder.
5) The waste water without the rubber powder is used as process water for preparing sodium sulfite solution and sodium hydroxide solution, and the residual 1.5t/h is subjected to debromination and recovery.
6) And (3) recycling the residual bromine-containing wastewater at 14t/h of about 80 ℃ in the step 3) as hot water in the step 2).
The amount of the gum ends in the waste water containing no gum ends obtained by hexane extraction was not reduced to a detectable level from 0.35wt%. The operation period of the bromine recovery equipment is prolonged to 1 year from the original 15 days; the waste water without rubber powder replaces fresh process water to prepare solution of sodium sulfite and other auxiliaries, and is used as machine seal washing water and the like, so that the consumption of the fresh process water is reduced, and the external discharge of the waste water is reduced.
Example 2
1) And (2) contacting bromine with a butyl rubber hexane solution to perform substitution reaction to obtain a hexane solution containing bromo-butyl rubber and hydrogen bromide, namely the bromo-butyl rubber reaction solution.
2') at 55 ℃, feeding 6700kg/h (containing 25.3kg/h of hydrogen bromide and 1020kg/h of bromobutyl rubber) of bromobutyl rubber reaction liquid into a packed tower from the lower part, and simultaneously feeding 1500kg/h of washing water and the bromobutyl rubber reaction liquid into the packed tower from the upper part of the packed tower to reversely contact with each other; 1520kg/h of bromide ion-containing water phase is obtained from the bottom of the packed tower; the bromobutyl rubber solution phase 6680kg/h is obtained at the top of the tower.
Adding 40kg/h 10% sodium sulfite aqueous solution into the bromobutyl rubber solution phase 6680kg/h obtained from the tower top, then neutralizing with sodium hydroxide solution until the pH is =9, putting the bromobutyl rubber glue solution after neutralization into a water precipitation and condensation unit to contact with water vapor of 2MPa and hot water of 75 ℃, and separating to obtain hexane solvent and brominated colloidal particle water.
3) And (3) dehydrating the brominated colloidal particles obtained in the step 2') to obtain the bromobutyl rubber and bromine-containing wastewater with the flow rate of about 16t/h and the temperature of 80 ℃.
4) Contacting the bromine-containing wastewater (with the content of the rubber powder of 0.35 wt%) of 0.5t/h in the step 3) with hexane of 0.25t/h in an extraction tower, removing the rubber powder in the bromine-containing wastewater, and carrying out phase separation to obtain bromine-containing wastewater without the rubber powder of 0.5 t/h.
5) The bromine-containing wastewater without the rubber powder is used as process water for preparing sodium sulfite solution, preparing sodium hydroxide solution and washing the process.
6) The bromine-containing wastewater in the step 3) is recycled as a partial substitute of hot water in the step 2') at 14t/h and about 80 ℃;1.5t/h of bromine-containing wastewater is recycled as the washing water in the step 2').
7) 1520kg/h of the aqueous bromide ion phase obtained in step 2') and 750kg/h of hexane were contacted in an extraction column at a temperature of 50 ℃ to obtain an aqueous bromide ion phase free from the gum powder by phase separation.
8) The aqueous bromide ion-containing phase, free of the gum dust, is sent to a bromine recovery unit for bromine recovery.
The content of the gel powder is not reduced to be measured from 0.35wt% by hexane extraction to obtain bromine-containing waste water without gel powder or bromine ion-containing water phase without gel powder. The operation period of the bromine recovery equipment is prolonged to 1 year from the original 15 days; the waste water without rubber powder replaces fresh process water to prepare solution of sodium sulfite and other auxiliaries, and is used as machine seal washing water and the like, so that the consumption of the fresh process water is reduced, and the external discharge of the waste water is reduced.
The embodiments of the present invention have been described above by way of example. However, the scope of the present invention is not limited to the above embodiments. Any modification, equivalent replacement, improvement and the like made by those skilled in the art within the spirit and principle of the present invention shall be included in the protection scope of the present invention.
Claims (10)
1. A method for preparing a brominated polymer, comprising the steps of:
1) Contacting the polymer solution with liquid bromine to obtain a brominated polymer solution;
2) Contacting the brominated polymer solution with hot water and water vapor, and separating to obtain brominated colloidal particle water and an organic solvent;
3) Dehydrating the brominated colloidal particle water obtained in the step 2) to obtain brominated polymer and bromine-containing wastewater;
4) Contacting at least one part of the bromine-containing wastewater obtained in the step 3) with an organic extractant to obtain bromine-containing wastewater without rubber powder;
5) The bromine-containing waste water without the rubber powder is used as process water and/or bromine is recovered;
6) The residual part of the bromine-containing wastewater obtained in the step 3) is reused as hot water in the step 2).
2. The method for preparing according to claim 1, characterized in that it comprises the steps of:
1) Contacting the polymer solution with liquid bromine to obtain a brominated polymer solution;
2') carrying out contact washing on the brominated polymer solution obtained in the step 1) and washing water, carrying out phase separation, obtaining a brominated polymer solution phase at the top and obtaining a bromide ion-containing water phase at the bottom;
contacting the bromopolymer solution phase with hot water and water vapor, and separating to obtain brominated colloidal particle water and an organic solvent;
3) Dehydrating the brominated colloidal particle water in the step 2') to obtain brominated polymer and bromine-containing wastewater;
4) Contacting at least a part of the bromine-containing wastewater obtained in the step 3) with an organic extractant to obtain bromine-containing wastewater without rubber powder;
5) The bromine-containing waste water without the crumb rubber is used as process water and/or for recovering bromine;
6) The remaining part of the bromine-containing waste water obtained in step 3) is recycled as hot water in step 2 ') and/or as washing water in step 2').
3. The method of manufacturing according to claim 2, further comprising the steps of:
7) Contacting the water phase containing bromide ions in the step 2') with an organic extractant to obtain the waste water containing bromide ions without rubber powder;
8) The bromine ion-containing wastewater without the gum dust in the step 7) is used for recovering bromine.
4. The production method according to any one of claims 1 to 3, wherein in the step 1), the polymer is at least one of butyl rubber, polybutadiene, and a styrene-butadiene copolymer; the brominated polymer is one or a mixture of brominated butyl rubber, brominated polybutadiene and brominated styrene-butadiene copolymer;
preferably, in step 1), the polymer solution is obtained by dissolving a polymer in an organic solvent.
Preferably, the organic solvent in the polymer solution of step 1) includes, but is not limited to, C4-C8 alkanes; is at least one of n-pentane, cyclopentane, hexane (which may be, for example, n-hexane, 2-methylpentane, 3-methylpentane, 2,3-dimethylbutane or 2,2-dimethylbutane), cyclohexane or n-heptane, or mixtures thereof.
5. The method according to claim 1 or 4, wherein a base and/or a reducing agent may be further added to the solution of the brominated polymer before the solution of the brominated polymer is contacted with the hot water and the steam in the step 2). For example, the brominated polymer solution may be contacted, reacted with a base and/or a reducing agent, and then contacted with hot water and steam. For another example, when the alkali and the reducing agent are added simultaneously, the reducing agent is added first, and then the alkali is added, so that the pH of the system is 5 to 13, preferably 8 to 9;
preferably, the base is a hydroxide, an alkali metal carbonate, or an alkali metal bicarbonate of an alkali metal or alkaline earth metal, and may be at least one of sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate, sodium bicarbonate, potassium bicarbonate, or the like; the reducing agent is used for reducing unreacted bromine in the brominated polymer solution and is alkali metal sulfite or pyrosulfite, such as sodium sulfite or sodium pyrosulfite;
preferably, the mass of the reducing agent is 0 to 0.1wt% of the mass of the bromobutyl rubber solution;
preferably, in the step 2), the temperature of the hot water is 50-100 ℃; the pressure of the water vapor is 0.2-4 MPa.
Preferably, in the step 2), the container for contacting the brominated polymer solution with hot water and water vapor comprises a tower, a kettle and a tank.
6. The process according to any one of claims 2 to 4, wherein in step 2'), before the brominated polymer solution phase is contacted with the hot water and steam, a base and/or a reducing agent may be further added to the brominated polymer solution phase. For example, the brominated polymer solution phase may be contacted, reacted with a base and/or a reducing agent, and then contacted with hot water and steam. For another example, when the alkali and the reducing agent are added simultaneously, the reducing agent is added first, and then the alkali is added, so that the pH of the system is 5 to 13, preferably 8 to 9;
preferably, the base is hydroxide, alkali metal carbonate or alkali metal bicarbonate of alkali metal or alkaline earth metal, and is at least one of sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate, sodium bicarbonate, potassium bicarbonate and the like; the reducing agent is used for reducing unreacted bromine in the brominated polymer solution, and is alkali metal sulfite or pyrosulfite, and is sodium sulfite or sodium pyrosulfite.
Preferably, the mass of the reducing agent is 0 to 0.1wt% of the mass of the bromobutyl rubber solution phase.
Preferably, in step 2'), the temperature of the hot water is 50 to 100 ℃; the pressure of the water vapor is 0.2-4 MPa.
Preferably, step 2') comprises: and (3) carrying out contact washing on the brominated polymer solution and washing water in a container, carrying out phase separation, obtaining a brominated polymer solution phase at the top and obtaining a bromide ion-containing water phase at the bottom. Wherein the brominated polymer solution phase is used in contact with hot water and water vapor.
Preferably, the container for contact washing of the brominated polymer solution and the washing water comprises a tower, a kettle and a tank.
Preferably, step 2') is specifically that the brominated polymer solution and washing water are contacted and washed in a washing tower, a brominated polymer solution phase is obtained at the tower top, and a bromide ion-containing water phase is obtained at the tower bottom; and (3) sequentially adding a reducing agent and alkali into the brominated polymer solution phase to ensure that the pH value of the system is 5-13, contacting the neutralized brominated polymer solution phase with hot water and water vapor, and separating to obtain brominated colloidal particle water and an organic solvent.
Illustratively, the mass ratio of the brominated polymer solution to the washing water is (1-6): 1.
Illustratively, the wash water is one of process water, lye, an aqueous solution containing a reducing agent, bromine-containing wastewater, or bromine-containing wastewater without fines.
Preferably, in step 2'), the container for contacting the brominated polymer solution phase with hot water and water vapor comprises a tower, a kettle and a tank.
7. The production method according to any one of claims 1 to 6, wherein the content of the crumb rubber in the bromine-containing wastewater of the step 3) is not more than 0.35% by weight.
Preferably, the gum powder comprises a brominated polymer.
8. The preparation method according to any one of claims 1 to 7, wherein in the step 4), the mass ratio of the bromine-containing wastewater to the organic extractant is 1 (0.1 to 1); the contact temperature is 20-100 ℃.
Preferably, in the step 4), the mass of the bromine-containing wastewater contacted with the organic extractant is 1 to 30wt% of the total mass of the bromine-containing wastewater.
Illustratively, the bromine-containing wastewater is contacted with the organic extractant in a container, and particularly, the contact container comprises a tower, a kettle and a tank.
9. The production method according to any one of claims 3 to 4 and 6 to 8, wherein in the step 7), the mass ratio of the bromide ion-containing aqueous phase to the organic extractant is 1 (0.1 to 1); the contact temperature is 20-100 ℃.
Preferably, in step 7), the bromide ion-containing aqueous phase is contacted with the organic extractant in its entirety.
Preferably, the organic extractant is an organic solvent in which the brominated polymer is dissolved, and the organic extractant contains 0 to 5 weight percent of the brominated polymer.
10. The production method according to any one of claims 1 to 9, wherein in step 6), the remaining portion of the bromine-containing wastewater is divided into two portions, 0 to 30wt% is used as the washing water in step 2 '), and 70 to 100% is reused as the hot water in step 2');
preferably, in step 6), the mass of the remaining portion of the bromine-containing wastewater is 70 to 97wt%, for example, 70 to 95wt%, and further for example, 80 to 90wt% of the total mass of the bromine-containing wastewater.
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