CN110614084A - Preparation method of composite adsorbent for wastewater treatment - Google Patents

Preparation method of composite adsorbent for wastewater treatment Download PDF

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Publication number
CN110614084A
CN110614084A CN201911070200.3A CN201911070200A CN110614084A CN 110614084 A CN110614084 A CN 110614084A CN 201911070200 A CN201911070200 A CN 201911070200A CN 110614084 A CN110614084 A CN 110614084A
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China
Prior art keywords
diatomite
chitosan
liquid
modified
composite adsorbent
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CN201911070200.3A
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Chinese (zh)
Inventor
朱康民
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Yunnan Xinxiang Green Environmental Technology Co Ltd
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Yunnan Xinxiang Green Environmental Technology Co Ltd
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Priority to CN201911070200.3A priority Critical patent/CN110614084A/en
Publication of CN110614084A publication Critical patent/CN110614084A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/14Diatomaceous earth
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/22Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
    • B01J20/24Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/28Treatment of water, waste water, or sewage by sorption
    • C02F1/288Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered

Abstract

The invention discloses a preparation method of a composite adsorbent for wastewater treatment, which comprises the following steps: (1) grinding diatomite; (2) adding concentrated sulfuric acid into the ground diatomite according to the liquid-solid ratio (g/mL) of 0.05-0.5:1, and carrying out modification treatment at the temperature of 65-85 ℃ for 15min-120min to obtain a modified mixed solution; (3) filtering the modified mixed solution, and drying the residue obtained after filtering to obtain modified diatomite; (4) dissolving chitosan in water, adding acetic acid to generate colloidal liquid, and adding modified diatomite into the colloidal liquid to obtain a blending liquid; adding a sodium hydroxide solution into the blending liquid to obtain flocculent precipitate; (5) and filtering, washing and drying the flocculent precipitate to obtain the chitosan-diatomite composite adsorbent. (2) The raw materials of diatomite, concentrated sulfuric acid and chitosan in the process are easy to obtain, the preparation process is simple, the production cost is low, the adsorption effect is good, and the process is particularly suitable for treating industrial wastewater.

Description

Preparation method of composite adsorbent for wastewater treatment
Technical Field
The invention relates to the technical field of water pollution treatment, in particular to a preparation method of a composite adsorbent for wastewater treatment.
Background
The chitosan and the derivatives thereof have good flocculation and clarification effects. As a clarifying agent of the beverage, the flocculant can quickly flocculate and naturally precipitate suspended matters, and improve the yield of stock solution; in the Chinese medicinal extractive solution, macromolecular protein, tannic acid and pectin can be conveniently removed with chitosan solution, and high-purity Chinese medicinal effective components are refined; the chitosan has good effect on water purification by utilizing the adsorbability of the chitosan.
Diatomite is siliceous rock which mainly comprises SiO2 as a chemical component, contains a small amount of Al2O3, Fe2O3, CaO, MgO and the like and organic matters, and mainly consists of remains of ancient diatoms. The diatomaceous earth can be observed under an electron microscope to have a particular porous structure. The diatomite is easy to obtain and low in price, and is widely applied to the field of sewage treatment.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a preparation method of a composite adsorbent for wastewater treatment, and the composite adsorbent prepared by the preparation method has a good adsorption effect.
In order to solve the technical problems, the technical scheme of the invention is as follows:
a preparation method of a composite adsorbent for wastewater treatment comprises the following steps:
(1) grinding diatomite;
(2) adding concentrated sulfuric acid into the ground diatomite according to the liquid-solid ratio (g/mL) of 0.05-0.5:1, and carrying out modification treatment at the temperature of 65-85 ℃ for 15min-120min to obtain a modified mixed solution;
(3) filtering the modified mixed solution, and drying the residue obtained after filtering to obtain modified diatomite;
(4) dissolving chitosan in water, adding acetic acid to generate colloidal liquid, and adding modified diatomite into the colloidal liquid to obtain a blending liquid; adding a sodium hydroxide solution into the blending liquid to obtain flocculent precipitate;
(5) and filtering, washing and drying the flocculent precipitate to obtain the chitosan-diatomite composite adsorbent.
Preferably, the modification treatment time in the step (1) is 30-60 min.
Preferably, the liquid-solid ratio (g/mL) in the step (1) is 0.2-0.25: 1.
Preferably, the mass ratio of the chitosan to the modified diatomite in the step (4) is 1: 2-10.
The preparation of the composite adsorbent comprises two processes: one is the modification process of diatomite, and the other is the modification process of chitosan. Because the diatomite mineral raw material contains capillary water and some organic matters, the modification is carried out by concentrated phosphoric acid, the strong dehydration property of the concentrated sulfuric acid can remove the capillary water, and the pore structure of the diatomite is improved, thereby improving the adsorption effect. The modified diatomite and the modified chitosan are compounded, and the effect of the compounded modified diatomite and the modified chitosan is to enhance the adsorption performance by utilizing the synergistic decontamination effect after compounding.
The invention has the beneficial effects that:
(1) by adopting the technical scheme, the diatomite is modified by utilizing the strong dehydration property of the concentrated sulfuric acid, so that capillary water in the diatomite can be removed, a pipeline is further dredged, and the pore area and the surface area are increased, so that the capability of the diatomite for adsorbing organic pollutants is effectively enhanced; after the modified diatomite and the modified chitosan are compounded, different kinds of pollutants can be selectively adsorbed, the sewage treatment range is enlarged, and meanwhile, the synergistic effect is better than that in single adsorption operation.
(2) The raw materials of diatomite, concentrated sulfuric acid and chitosan in the process are easy to obtain, the preparation process is simple, the production cost is low, the adsorption effect is good, and the process is particularly suitable for treating industrial wastewater.
Detailed Description
The following examples further illustrate embodiments of the present invention. It should be noted that the description of the embodiments is provided to help understanding of the present invention, but the present invention is not limited thereto. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
Example 1
A preparation method of a composite adsorbent for wastewater treatment comprises the following steps:
(1) grinding 200g of diatomite;
(2) transferring the ground diatomite into a beaker, adding 1000ml of 98% concentrated sulfuric acid, and carrying out modification treatment for 120min under the water bath heating condition of 65 ℃ to obtain a modified mixed solution;
(3) filtering the modified mixed solution, and drying the residue obtained after filtering to obtain modified diatomite;
(4) dissolving 20g of chitosan in water, adding 5ml of acetic acid with the mass concentration of 95% into the chitosan to generate colloidal liquid, and adding the modified diatomite obtained in the step (3) into the colloidal liquid to obtain blended liquid; adding a sodium hydroxide solution into the blending liquid to obtain flocculent precipitate;
(5) and filtering, washing and drying the flocculent precipitate to obtain the chitosan-diatomite composite adsorbent.
And (3) sewage treatment test: taking 1000ml of industrial wastewater of a certain paper mill in south, wherein the COD content of the wastewater is 336.07mg/L, the pH value is 6-7, adding 3.5g of the chitosan-diatomite composite adsorbent into the industrial wastewater, uniformly stirring, standing at 50 ℃ for 60min, and obtaining a treated solution with the COD content of 37.05mg/L and the removal rate of 88.98%.
Example 2
A preparation method of a composite adsorbent for wastewater treatment comprises the following steps:
(1) grinding 250g of diatomite;
(2) transferring the ground diatomite into a beaker, adding 1000ml of 98% concentrated sulfuric acid, and carrying out modification treatment for 15min under the water bath heating condition of 85 ℃ to obtain a modified mixed solution;
(3) filtering the modified mixed solution, and drying the residue obtained after filtering to obtain modified diatomite;
(4) dissolving 50g of chitosan in water, adding 10ml of acetic acid with the mass concentration of 95% into the chitosan to generate colloidal liquid, and adding the modified diatomite obtained in the step (3) into the colloidal liquid to obtain blended liquid; adding a sodium hydroxide solution into the blending liquid to obtain flocculent precipitate;
(5) and filtering, washing and drying the flocculent precipitate to obtain the chitosan-diatomite composite adsorbent.
And (3) sewage treatment test: taking 1000ml of industrial wastewater of a certain paper mill in south, wherein the COD content of the wastewater is 382.36mg/L, the pH value is 6-7, adding 4g of the chitosan-diatomite composite adsorbent into the industrial wastewater, uniformly stirring, standing at 60 ℃ for 45min, and obtaining a solution with the COD content of 40.53mg/L and the removal rate of 89.40%.
Example 3
A preparation method of a composite adsorbent for wastewater treatment comprises the following steps:
(1) grinding 100g of diatomite;
(2) transferring the ground diatomite into a beaker, adding 1000ml of 98% concentrated sulfuric acid, and carrying out modification treatment for 60min under the water bath heating condition of 65 ℃ to obtain a modified mixed solution;
(3) filtering the modified mixed solution, and drying the residue obtained after filtering to obtain modified diatomite;
(4) dissolving 100g of chitosan in water, adding 8ml of acetic acid with the mass concentration of 95% into the chitosan to generate colloidal liquid, and adding the modified diatomite obtained in the step (3) into the colloidal liquid to obtain blended liquid; adding a sodium hydroxide solution into the blending liquid to obtain flocculent precipitate;
(5) and filtering, washing and drying the flocculent precipitate to obtain the chitosan-diatomite composite adsorbent.
And (3) sewage treatment test: taking 1000ml of industrial wastewater of a certain rubber factory in south, wherein the COD content of the wastewater is 277.49mg/L, the pH value is 6-7, adding 5g of the chitosan-diatomite composite adsorbent into the industrial wastewater, uniformly stirring, standing at 55 ℃ for 60min, and obtaining a treated solution with the COD content of 25.46mg/L and the removal rate of 90.82%.
Example 4
A preparation method of a composite adsorbent for wastewater treatment comprises the following steps:
(1) grinding 500g of diatomite;
(2) transferring the ground diatomite into a beaker, adding 1000ml of 98% concentrated sulfuric acid, and carrying out modification treatment for 120min under the water bath heating condition of 75 ℃ to obtain a modified mixed solution;
(3) filtering the modified mixed solution, and drying the residue obtained after filtering to obtain modified diatomite;
(4) dissolving 50g of chitosan in water, adding 10ml of acetic acid with the mass concentration of 95% into the chitosan to generate colloidal liquid, and adding the modified diatomite obtained in the step (3) into the colloidal liquid to obtain blended liquid; adding a sodium hydroxide solution into the blending liquid to obtain flocculent precipitate;
(5) and filtering, washing and drying the flocculent precipitate to obtain the chitosan-diatomite composite adsorbent.
And (3) sewage treatment test: taking 1000ml of industrial wastewater of a certain rubber factory in south, wherein the COD content of the wastewater is 293.65mg/L, the pH value is 6-7, adding 4.5g of the chitosan-diatomite composite adsorbent into the industrial wastewater, uniformly stirring, standing at 65 ℃ for 30min, and obtaining a treated solution with the COD content of 28.35mg/L and the removal rate of 90.35%.
The embodiments of the present invention have been described in detail with reference to the examples, but the present invention is not limited to the described embodiments. It will be apparent to those skilled in the art that various changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, and the scope of protection is still within the scope of the invention.

Claims (4)

1. A preparation method of a composite adsorbent for wastewater treatment is characterized by comprising the following steps:
(1) grinding diatomite;
(2) adding concentrated sulfuric acid into the ground diatomite according to the liquid-solid ratio (g/mL) of 0.05-0.5:1, and carrying out modification treatment at the temperature of 65-85 ℃ for 15min-120min to obtain a modified mixed solution;
(3) filtering the modified mixed solution, and drying the residue obtained after filtering to obtain modified diatomite;
(4) dissolving chitosan in water, adding acetic acid to generate colloidal liquid, and adding modified diatomite into the colloidal liquid to obtain a blending liquid; adding a sodium hydroxide solution into the blending liquid to obtain flocculent precipitate;
(5) and filtering, washing and drying the flocculent precipitate to obtain the chitosan-diatomite composite adsorbent.
2. The method for preparing the composite adsorbent for wastewater treatment according to claim 1, wherein the modification treatment time in the step (1) is 30-60 min.
3. The method for preparing the composite adsorbent for wastewater treatment according to claim 1, wherein the liquid-solid ratio (g/mL) in the step (1) is 0.2-0.25: 1.
4. The method for preparing the composite adsorbent for wastewater treatment according to claim 1, wherein the mass ratio of the chitosan to the modified diatomite in the step (4) is 1: 2-10.
CN201911070200.3A 2019-11-05 2019-11-05 Preparation method of composite adsorbent for wastewater treatment Pending CN110614084A (en)

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Cited By (5)

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Publication number Priority date Publication date Assignee Title
CN111320347A (en) * 2020-03-16 2020-06-23 武夷学院 Treatment method of secondary sedimentation tank sludge of domestic sewage plant
CN111514847A (en) * 2020-05-15 2020-08-11 辽宁科隆精细化工股份有限公司 Preparation method of modified diatomite and application of modified diatomite in salt-containing wastewater treatment
CN112007610A (en) * 2020-09-04 2020-12-01 桂林良物造日用品有限公司 Preparation method of diatomite-coated nano white carbon material with high adsorption performance
CN112723554A (en) * 2020-11-05 2021-04-30 云南锦淮环保科技有限公司 Composite biological water purifying agent and preparation method thereof
CN113072075A (en) * 2021-03-30 2021-07-06 湖南三友环保科技有限公司 Preparation method and application of sulfur-based diatomite powder material

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111320347A (en) * 2020-03-16 2020-06-23 武夷学院 Treatment method of secondary sedimentation tank sludge of domestic sewage plant
CN111514847A (en) * 2020-05-15 2020-08-11 辽宁科隆精细化工股份有限公司 Preparation method of modified diatomite and application of modified diatomite in salt-containing wastewater treatment
CN111514847B (en) * 2020-05-15 2023-09-08 辽宁科隆精细化工股份有限公司 Preparation method of modified diatomite and application of modified diatomite in treatment of saline wastewater
CN112007610A (en) * 2020-09-04 2020-12-01 桂林良物造日用品有限公司 Preparation method of diatomite-coated nano white carbon material with high adsorption performance
CN112723554A (en) * 2020-11-05 2021-04-30 云南锦淮环保科技有限公司 Composite biological water purifying agent and preparation method thereof
CN112723554B (en) * 2020-11-05 2023-02-28 云南锦淮环保科技有限公司 Composite biological water purifying agent and preparation method thereof
CN113072075A (en) * 2021-03-30 2021-07-06 湖南三友环保科技有限公司 Preparation method and application of sulfur-based diatomite powder material

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