CN112742356B - Adsorption resin for treating waste water and gas and preparation method thereof - Google Patents
Adsorption resin for treating waste water and gas and preparation method thereof Download PDFInfo
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
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- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
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Abstract
The invention provides an adsorption resin for treating wastewater and waste gas, which is prepared from the following raw materials in parts by weight: 850-950 parts of dry white balls, 700-850 parts of catalysts, 805-855 parts of chloromethylation reagents, 3500-3600 parts of solvents and 2000 parts of water. The invention also provides a preparation method of the adsorption resin for treating wastewater and waste gas. The adsorption resin for treating wastewater and waste gas provided by the invention uses less chloromethyl ether, has lower production cost and better performance.
Description
Technical Field
The invention relates to a resin, in particular to an adsorption resin for treating waste water and waste gas and a preparation method thereof.
Background
The adsorption resin is a special macroporous resin, takes adsorption as a basic characteristic, mostly has no functional group but no exchange center, has the similar action as adsorbent activated carbon, can be regenerated, and is very suitable for treating waste water and waste gas. The existing preparation process of the adsorption resin generally comprises the following steps:
the first step is as follows: chlorination reaction
Raw materials: 900kg of dry white ball, 27 bags of zinc chloride, 4140L of chloromethyl ether and 5000L of reaction kettle
The operation is as follows: adding chloromethyl ether into the dry white balls, stirring and expanding for 2 hours, adding 13 bags of zinc chloride, opening a jacket, cooling for half an hour, adding secondary zinc chloride, closing cooling water, stirring for half an hour, heating to 43 ℃, keeping the temperature for 16 hours, cooling and sampling until the temperature is more than 17.5, filtering mother liquor, adding water, washing to be neutral, discharging, and drying for later use.
The second step is that: post-crosslinking reaction
Raw materials: 1000kg of dry chlorine ball, 220kg of aluminum trichloride (4 bags and half bags) and 3.5 tons of dichloroethane
The operation is as follows: adding dichloroethane into the dry chlorine ball, stirring and expanding for 2 hours, adding 2 bags of aluminum trichloride, stirring for half an hour, slowly heating to 80 +/-1 ℃, keeping the temperature for 1 hour, cooling to below 40 ℃, adding secondary aluminum trichloride, stirring, slowly heating to 80 +/-1 ℃, keeping the temperature for 3 hours, cooling, detecting that the residual chlorine content is less than 3%, adding water, boiling the ball, continuously heating to above 90 ℃ for 6 hours (supplementing a small amount of water for many times midway), decompressing for 1 hour, opening, cooling and washing after a user smells that the outlet is basically odorless.
The preparation method has the problems that the dosage of chloromethyl ether is large, the production cost is increased, the toxicity is large, potential safety hazards exist for production personnel, in addition, the preparation procedures are more, the operation is complex, the production cost is high, and the performance of the prepared adsorption resin is not ideal.
Chinese patent application CN200610087446.8 discloses a method for preparing an adsorption material, wherein the adsorption material is a highly crosslinked macroporous adsorption resin prepared by chloromethylation and additional crosslinking reaction by using a terpolymer of highly crosslinked macroporous polystyrene, vinyl acetate and divinylbenzene as a framework; the preparation method comprises the following steps: copolymerization, chloromethylation reaction and additional crosslinking reaction to produce the product of homogeneous pore netted high crosslinked macroporous adsorption resin. The invention is similar to the existing preparation method, and has the same problems: the dosage of chloromethyl ether is large, the preparation procedures are more, the operation is complex, the production cost is high, and the performance of the adsorption resin is not ideal.
Disclosure of Invention
The invention aims to provide an adsorption resin for treating wastewater and waste gas, which uses less chloromethyl ether, has lower production cost and better performance.
In order to solve the technical problems, the technical scheme of the invention is as follows:
an adsorption resin for treating wastewater and waste gas is prepared from the following raw materials in parts by weight: 850-950 parts of dry white balls, 700-850 parts of catalysts, 805-855 parts of chloromethylation reagents, 3500-3600 parts of solvents and 2000 parts of water.
Further, the catalyst of the invention is zinc chloride.
Further, the chloromethylation reagent is chloromethyl ether.
Further, the solvent of the present invention is dichloroethane.
The invention also provides a preparation method of the adsorption resin for treating wastewater and waste gas.
In order to solve the technical problems, the technical scheme is as follows:
a preparation method of an adsorption resin for treating wastewater and waste gas comprises the following steps:
s1, weighing the raw materials in parts by weight, putting dry white balls, a solvent and 4/5 weight of catalyst into a reactor, and swelling for 1-3 hours at normal temperature;
s2, adding a chloromethylation reagent into a reactor, heating to 39-41 ℃, and then preserving heat for 15-17 hours;
s3, adding the remaining catalyst into a reactor, heating to 79-81 ℃, and then preserving heat for 3-5 hours to obtain a first crude ball;
s4, sampling and inspecting, namely adding 3/4 weight of water into a reactor when the residual chlorine content of the inspected crude ball I is lower than 3%, heating to 90-100 ℃, and evaporating to remove the solvent to obtain a crude ball II;
and S5, washing the coarse balls with the remaining water until the pH value of the coarse balls is 4-6, discharging and packaging to obtain the finished product of the adsorption resin for treating the waste water and the waste gas.
Further, the reactor of the present invention is a jet loop reactor.
Further, in step S1 of the present invention, the swelling time at room temperature is 2 hours.
Further, in step S2 of the present invention, the heat preservation time is 16 hours.
Further, in step S3 of the present invention, the heat preservation time is 4 hours.
Compared with the prior art, the invention has the following beneficial effects:
1) the amount of the chloromethyl ether used in the invention is only about 20 percent of that in the existing preparation process, thereby effectively reducing the production cost and the potential safety hazard to production personnel.
2) Compared with the existing preparation process, the method does not need to dry the chlorine balls, simplifies the production process, is more convenient to operate, and further reduces the production cost.
3) The reactor used in the invention is a jet loop reactor, which can effectively improve the adsorption performance and stability of the adsorption resin.
4) In the preparation process of the invention, the catalyst is added in stages, namely 4/5 weight of catalyst is added in step S1, and then the rest catalyst is added in step S3, so that the reaction degree can be effectively improved, and the heat resistance and the strength of the adsorption resin are further improved.
Detailed Description
The present invention will be described in detail with reference to specific embodiments, and the exemplary embodiments and descriptions thereof herein are provided to explain the present invention but not to limit the present invention.
Example 1
The adsorption resin for treating waste water and waste gas is prepared from the following raw materials in parts by weight: 900 parts of dry white balls, 770 parts of zinc chloride, 828 parts of chloromethyl ether, 3550 parts of dichloroethane and 2000 parts of water.
The preparation method of the adsorption resin for treating wastewater and waste gas comprises the following steps:
s1, weighing the raw materials in parts by weight, putting dry white balls, dichloroethane and 4/5 parts by weight of zinc chloride into a jet loop reactor, and swelling for 2 hours at normal temperature;
s2, adding chloromethyl ether into a jet loop reactor, heating to 40 ℃, and then preserving heat for 16 hours;
s3, adding the remaining zinc chloride into a jet loop reactor, heating to 80 ℃, and then preserving heat for 4 hours to obtain a first crude ball;
s4, sampling and inspecting, namely adding 3/4 weight of water into a jet loop reactor when the residual chlorine content of the inspected crude ball I is lower than 3%, heating to 95 ℃, and distilling off dichloroethane, thus obtaining a crude ball II after the dichloroethane is distilled off;
and S5, washing the coarse balls with the remaining water until the pH value of the coarse balls is 5, discharging and packaging to obtain the finished product of the adsorption resin for treating the waste water and the waste gas.
Example 2
The adsorption resin for treating waste water and waste gas is prepared from the following raw materials in parts by weight: 850 parts of dry white balls, 700 parts of zinc chloride, 805 parts of chloromethyl ether, 3500 parts of dichloroethane and 2000 parts of water.
The preparation method of the adsorption resin for treating wastewater and waste gas comprises the following steps:
s1, weighing the raw materials in parts by weight, putting dry white balls, dichloroethane and 4/5 parts by weight of zinc chloride into a jet loop reactor, and swelling for 1 hour at normal temperature;
s2, adding chloromethyl ether into a jet loop reactor, heating to 39 ℃, and then preserving heat for 17 hours;
s3, adding the remaining zinc chloride into a jet loop reactor, heating to 79 ℃, and then preserving heat for 5 hours to obtain a crude ball I;
s4, sampling and inspecting, namely adding 3/4 weight of water into a jet loop reactor when the residual chlorine content of the inspected crude ball I is lower than 3%, heating to 90 ℃, and then distilling off dichloroethane, thus obtaining a crude ball II after the dichloroethane is distilled off;
and S5, washing the coarse balls with the remaining water until the pH value of the coarse balls is 6, discharging and packaging to obtain the finished product of the adsorption resin for treating the waste water and the waste gas.
Example 3
The adsorption resin for treating waste water and waste gas is prepared from the following raw materials in parts by weight: 950 parts of dry white balls, 850 parts of zinc chloride, 855 parts of chloromethyl ether, 3600 parts of dichloroethane and 2000 parts of water.
The preparation method of the adsorption resin for treating wastewater and waste gas comprises the following steps:
s1, weighing the raw materials in parts by weight, putting dry white balls, dichloroethane and 4/5 parts by weight of zinc chloride into a jet loop reactor, and swelling for 3 hours at normal temperature;
s2, adding chloromethyl ether into a jet loop reactor, heating to 41 ℃, and then preserving heat for 15 hours;
s3, adding the remaining zinc chloride into a jet loop reactor, heating to 81 ℃, and then preserving heat for 3 hours to obtain a crude ball I;
s4, sampling and inspecting, namely adding water in an amount of 3/4 weight into a jet loop reactor when the residual chlorine content of the inspected crude ball I is lower than 3%, heating to 100 ℃, and then distilling off dichloroethane, thus obtaining a crude ball II after the dichloroethane is distilled off;
and S5, washing the coarse balls with the remaining water until the pH value of the coarse balls is 4, discharging and packaging to obtain the finished product of the adsorption resin for treating the waste water and the waste gas.
Example 4
The adsorption resin for treating waste water and waste gas is prepared from the following raw materials in parts by weight: 920 parts of dry white balls, 810 parts of zinc chloride, 840 parts of chloromethyl ether, 3570 parts of dichloroethane and 2000 parts of water.
The preparation method of the adsorption resin for treating wastewater and waste gas comprises the following steps:
s1, weighing the raw materials in parts by weight, putting dry white balls, dichloroethane and 4/5 parts by weight of zinc chloride into a jet loop reactor, and swelling for 1.5 hours at normal temperature;
s2, adding chloromethyl ether into a jet loop reactor, heating to 39 ℃, and then preserving heat for 16 hours;
s3, adding the remaining zinc chloride into a jet loop reactor, heating to 80 ℃, and then preserving heat for 5 hours to obtain a crude ball I;
s4, sampling and inspecting, namely adding water 3/4 in weight into a jet loop reactor when the residual chlorine content of the inspected crude ball I is lower than 3%, heating to 92 ℃, and distilling off dichloroethane, thus obtaining a crude ball II after the dichloroethane is distilled off;
and S5, washing the coarse balls with the remaining water until the pH value of the coarse balls is 4.5, discharging and packaging to obtain the finished product of the adsorption resin for treating the waste water and the waste gas.
Reference example 1:
the adsorption resin for treating waste water and waste gas is prepared from the following raw materials in parts by weight: 900 parts of dry white balls, 770 parts of zinc chloride, 828 parts of chloromethyl ether, 3550 parts of dichloroethane and 2000 parts of water.
The preparation method of the adsorption resin for treating wastewater and waste gas comprises the following steps:
s1, weighing the raw materials in parts by weight, putting dry white balls, dichloroethane and 4/5 parts by weight of zinc chloride into a reaction kettle, and swelling for 2 hours at normal temperature;
s2, adding chloromethyl ether into a reaction kettle, heating to 40 ℃, and then preserving heat for 16 hours;
s3, adding the remaining zinc chloride into a reaction kettle, heating to 80 ℃, and then preserving heat for 4 hours to obtain a crude ball I;
s4, sampling and inspecting, namely adding 3/4 weight of water into the reaction kettle when the residual chlorine content of the inspected crude ball I is lower than 3%, heating to 95 ℃, and distilling off dichloroethane, thus obtaining a crude ball II after the dichloroethane is distilled off;
and S5, washing the coarse balls with the remaining water until the pH value of the coarse balls is 5, discharging and packaging to obtain the finished product of the adsorption resin for treating the waste water and the waste gas.
Reference example 1 differs from example 1 in that: the jet loop reactor in the preparation method is replaced by a common reaction kettle.
Reference example 2:
the adsorption resin for treating waste water and waste gas is prepared from the following raw materials in parts by weight: 900 parts of dry white balls, 770 parts of zinc chloride, 828 parts of chloromethyl ether, 3550 parts of dichloroethane and 2000 parts of water.
The preparation method of the adsorption resin for treating wastewater and waste gas comprises the following steps:
s1, weighing the raw materials in parts by weight, putting dry white balls, dichloroethane and zinc chloride into a jet loop reactor, and swelling for 2 hours at normal temperature;
s2, adding chloromethyl ether into a jet loop reactor, heating to 40 ℃, then preserving heat for 16 hours, heating to 80 ℃, and preserving heat for 4 hours to obtain a crude ball I;
s3, sampling and inspecting, namely adding water in an amount of 3/4 weight into a jet loop reactor when the residual chlorine content of the inspected crude ball I is lower than 3%, heating to 95 ℃, and then distilling off dichloroethane, thus obtaining a crude ball II after the dichloroethane is distilled off;
and S4, washing the coarse balls with the remaining water until the pH value of the coarse balls is 5, discharging and packaging to obtain the finished product of the adsorption resin for treating the waste water and the waste gas.
The difference from example 1 is that: the zinc chloride is added all at once to the jet loop reactor in step S1. Reference example 3:
the adsorption resin for treating waste water and waste gas is prepared from the following raw materials in parts by weight: 900 parts of dry white balls, 770 parts of zinc chloride, 828 parts of chloromethyl ether, 3550 parts of dichloroethane and 2000 parts of water.
The preparation method of the adsorption resin for treating wastewater and waste gas comprises the following steps:
s1, weighing the raw materials in parts by weight, putting dry white balls and dichloroethane into a jet loop reactor, and swelling for 2 hours at normal temperature;
s2, adding chloromethyl ether into a jet loop reactor, heating to 40 ℃, and then preserving heat for 16 hours;
s3, adding zinc chloride into the jet loop reactor, heating to 80 ℃, and then preserving heat for 4 hours to obtain a first crude ball;
s4, sampling and inspecting, namely adding 3/4 weight of water into a jet loop reactor when the residual chlorine content of the inspected crude ball I is lower than 3%, heating to 95 ℃, and distilling off dichloroethane, thus obtaining a crude ball II after the dichloroethane is distilled off;
and S5, washing the coarse balls with the remaining water until the pH value of the coarse balls is 5, discharging and packaging to obtain the finished product of the adsorption resin for treating the waste water and the waste gas.
The difference from example 1 is that: the zinc chloride is added all at once to the jet loop reactor in step S3. Comparative example: example 1 of chinese patent application No. CN 200610087446.8.
Test example 1: adsorption Performance test
The test method comprises the following steps: the adsorbent resins of examples 1 to 4, reference examples 1 to 3 and comparative example were each added to 25mL of an aqueous benzyl alcohol solution, and the mass concentration of the aqueous benzyl alcohol solution was measured after shaking for 3 hours. The static adsorption capacity of the adsorption resin to the benzyl alcohol is calculated according to the following formula:
Q1=(C2-C1)·V/m
wherein Q is1Is the static adsorption capacity, mg/g; c2The mass concentration of the benzyl alcohol in the benzyl alcohol aqueous solution before adsorption is mg/L; c1The mass concentration of the benzyl alcohol in the adsorbed benzyl alcohol water solution is mg/L; v is the volume of the benzyl alcohol aqueous solution, L; m is the mass of the adsorbent resin, g.
Q1The larger the size, the better the adsorption performance, and the test results are shown in table 1:
Q1(mg/g) | |
example 1 | 606.59 |
Example 2 | 602.78 |
Example 3 | 604.27 |
Example 4 | 605.46 |
Reference example 1 | 538.64 |
Reference example 2 | 606.57 |
Reference example 3 | 606.56 |
Comparative example | 535.85 |
TABLE 1
As can be seen from Table 1, Q of examples 1 to 4 of the present invention1All the adsorption resins are larger than the comparative examples, which shows that the adsorption resin for treating wastewater and waste gas has better adsorption performance. Reference examples 1 to 3 the procedures for the preparation of reference examples 1 to 3 are partially different from those in example 1, Q of reference example 11The reduction shows that the jet circulation reactor used in the invention can effectively improve the adsorption resinAnd (4) adsorption performance.
Test example 2: stability test
The test method comprises the following steps: examples 1 to 4, reference examples 1 to 3, and comparative example were each repeated 20 times by repeating the method of test example 1, rinsing with deionized water and dilute hydrochloric acid after each adsorption, and the amount of static adsorption Q after 20 repetitions was determined2The static adsorption amount change rate was calculated according to the following formula:
δ=∣Q2-Q1∣/Q1×100%
wherein, δ is the static adsorption capacity change rate,%; q1The amount of the adsorbed water was mg/g, which was the amount of the adsorbed water measured in test example 1; q2The amount of adsorbed water was mg/g, which was the amount of static adsorption measured in test example 2.
Lower δ indicates better stability, and the test results are shown in table 2:
δ(%) | |
example 1 | 1.24 |
Example 2 | 1.26 |
Example 3 | 1.29 |
Example 4 | 1.28 |
Reference example 1 | 1.95 |
Reference example 2 | 1.25 |
Reference example 3 | 1.24 |
Comparative example | 1.97 |
TABLE 2
As can be seen from Table 2, the delta values of examples 1 to 4 of the present invention are all lower than those of the comparative examples, indicating that the adsorbent resin for treating waste water and exhaust gas according to the present invention has better stability. Reference examples 1 to 3 were partially different from example 1 in the operation, and the delta of reference example 1 was increased, which shows that the jet loop reactor used in the present invention is effective for improving the stability of the adsorption resin.
Test example 3: heat resistance test
The test method comprises the following steps: initial decomposition temperatures of examples 1 to 4, reference examples 1 to 3 and comparative example were measured by thermogravimetric analyzer at a temperature rising rate of 20 ℃ per minute and a temperature rising process from room temperature to 600 ℃. Higher initial decomposition temperature indicates better heat resistance, and the test results are shown in table 3:
initial decomposition temperature (. degree. C.) | |
Example 1 | 375.8 |
Example 2 | 375.5 |
Example 3 | 375.3 |
Example 4 | 375.6 |
Reference example 1 | 375.8 |
Reference example 2 | 358.4 |
Reference example 3 | 358.9 |
Comparative example | 361.2 |
TABLE 3
As can be seen from Table 3, the initial decomposition temperatures of examples 1 to 4 of the present invention were all higher than those of the comparative examples, indicating that the adsorbent resin for treating waste water and exhaust gas of the present invention has better heat resistance. The partial operations in the preparation methods of reference examples 1 to 3 are different from those in example 1, and the initial decomposition temperatures of reference examples 2 and 3 are both lowered, which shows that the stepwise addition operation of the catalyst in the preparation method of the present invention is effective in improving the heat resistance of the adsorbent resin.
Test example 4: strength test
The test method comprises the following steps: respectively carrying out drying on examples 1-4 and reference examples 1-3 and comparative examples, screening 50mL of spherical adsorbent resin balls out of a net, drying at 80 ℃ until the weight loss rate is below 3 wt%, cooling to room temperature, adding 100mL of absolute ethyl alcohol, stirring for 5 minutes, filtering to dry, separating the spherical adsorbent resin balls from fragments, respectively drying at 80 ℃ for 2 hours, weighing, and calculating the breakage rate according to the following formula:
the breaking rate is the weight of the fragments/(the weight of the spherical adsorbent resin and the weight of the fragments) × 100%
Lower breakage indicates higher strength and the test results are shown in table 4:
TABLE 4
As can be seen from Table 4, the breakage rates of examples 1 to 4 of the present invention were all lower than those of the comparative examples, indicating that the adsorbent resin for treating waste water and exhaust gas according to the present invention has a higher strength. The partial operations in the preparation methods of reference examples 1 to 3 are different from those in example 1, and the breakage rates of reference examples 2 and 3 are increased, which shows that the step-wise addition of the catalyst in the preparation method of the present invention is effective in improving the strength of the adsorbent resin.
The foregoing embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the invention. Any person skilled in the art can modify or change the above-mentioned embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention.
Claims (4)
1. An adsorption resin for treating waste water and waste gas is characterized in that: the feed is prepared from the following raw materials in parts by weight: 850-950 parts of dry white balls, 700-850 parts of catalysts, 805-855 parts of chloromethylation reagents, 3500-3600 parts of solvents and 2000 parts of water; the catalyst is zinc chloride, and the chloromethylation reagent is chloromethyl ether; the solvent is dichloroethane;
the preparation method of the adsorption resin for treating wastewater and waste gas comprises the following steps:
s1, weighing the raw materials in parts by weight, putting dry white balls, a solvent and 4/5 weight of catalyst into a jet loop reactor, and swelling for 1-3 hours at normal temperature;
s2, adding a chloromethylation reagent into the jet loop reactor, heating to 39-41 ℃, and then preserving heat for 15-17 hours;
s3, adding the remaining catalyst into a jet loop reactor, heating to 79-81 ℃, and then preserving heat for 3-5 hours to obtain a first crude ball;
s4, sampling and inspecting, namely adding 3/4 weight of water into a reactor when the residual chlorine content of the inspected crude ball I is lower than 3%, heating to 90-100 ℃, and evaporating to remove the solvent to obtain a crude ball II;
and S5, washing the coarse balls with the remaining water until the pH value of the coarse balls is 4-6, discharging and packaging to obtain the finished product of the adsorption resin for treating the waste water and the waste gas.
2. The adsorption resin for treating waste water and gas as claimed in claim 1, wherein: in step S1, the swelling time at room temperature was 2 hours.
3. The adsorption resin for treating waste water and gas as claimed in claim 1, wherein: in step S2, the heat-insulating time is 16 hours.
4. The adsorption resin for treating waste water and gas as claimed in claim 1, wherein: in step S3, the heat-insulating time is 4 hours.
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