CN114471462A - Efficient composite phosphorus removal agent and preparation method thereof - Google Patents

Efficient composite phosphorus removal agent and preparation method thereof Download PDF

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Publication number
CN114471462A
CN114471462A CN202210117530.9A CN202210117530A CN114471462A CN 114471462 A CN114471462 A CN 114471462A CN 202210117530 A CN202210117530 A CN 202210117530A CN 114471462 A CN114471462 A CN 114471462A
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composite phosphorus
removing agent
phosphorus removing
mixing
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胡昕
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Hunan Haishu Environmental Protection Technology Co ltd
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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
    • B01J20/04Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
    • B01J20/043Carbonates or bicarbonates, e.g. limestone, dolomite, aragonite
    • 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
    • B01J20/0203Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
    • B01J20/0225Compounds of Fe, Ru, Os, Co, Rh, Ir, Ni, Pd, Pt
    • B01J20/0229Compounds of Fe
    • 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
    • B01J20/0203Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
    • B01J20/0248Compounds of B, Al, Ga, In, Tl
    • 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
    • B01J20/0203Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
    • B01J20/0274Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04 characterised by the type of anion
    • B01J20/0288Halides of compounds other than those provided for in B01J20/046
    • 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
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/20Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
    • 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
    • C02F1/281Treatment of water, waste water, or sewage by sorption using inorganic sorbents
    • 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
    • C02F1/283Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2220/00Aspects relating to sorbent materials
    • B01J2220/40Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/48Sorbents characterised by the starting material used for their preparation
    • B01J2220/4812Sorbents characterised by the starting material used for their preparation the starting material being of organic character
    • B01J2220/485Plants or land vegetals, e.g. cereals, wheat, corn, rice, sphagnum, peat moss
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2220/00Aspects relating to sorbent materials
    • B01J2220/40Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/48Sorbents characterised by the starting material used for their preparation
    • B01J2220/4875Sorbents characterised by the starting material used for their preparation the starting material being a waste, residue or of undefined composition
    • B01J2220/4881Residues from shells, e.g. eggshells, mollusk shells
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/10Inorganic compounds
    • C02F2101/105Phosphorus compounds

Abstract

The invention discloses a high-efficiency composite phosphorus removal agent and a preparation method thereof, comprising the following steps of firstly, weighing raw materials; crushing the aggregate; step three, dissolving and extracting; step four, mixing and emulsifying; step five, drying at high temperature; step six, carbonizing the biological material; step seven, crushing and mixing; step eight, ultrasonic treatment; step nine, drying and packaging; according to the invention, coconut shells, straws and dead wood are carbonized and then added into the composite phosphorus removing agent, the carbonized material has rich pores and large specific surface area, the adsorption effect of the composite phosphorus removing agent is improved, other harmful substances are removed while phosphorus is removed, calcium ions in shells, pig bones and cow bones are extracted by hydrochloric acid to obtain soluble calcium ions, the calcium ions are easy to be synthesized into insoluble substances with phosphorus elements, and the insoluble substances are matched with polymeric ferric chloride and polymeric aluminum chloride for use, so that the phosphorus removing effect and efficiency of the composite phosphorus removing agent are enhanced.

Description

Efficient composite phosphorus removal agent and preparation method thereof
Technical Field
The invention relates to the technical field of chemical industry, in particular to a high-efficiency composite phosphorus removing agent and a preparation method thereof.
Background
The phosphorus removing agent is an article for coagulation turbidity removal treatment and phosphorus removal of urban water source water, can achieve the aim of deep phosphorus removal while performing coagulation turbidity removal treatment on the urban water source water, reduces the phosphorus content in the treated drinking water to be below a threshold value, does not need to change a raw water treatment process, does not need to add a large water treatment structure, is simple, convenient, practical, and can obtain remarkable social and economic benefits.
At present, phosphorus removing agents on the market are various in types, and can meet the use requirements of people, but certain defects still exist, the phosphorus removing effect of the phosphorus removing agents on the market is poor, the phosphorus removing efficiency is low, the purpose of removing phosphorus can be achieved by adding a large amount of phosphorus removing agents, the existing phosphorus removing agents have the phosphorus removing effect alone, the phosphorus removing agents do not have the phosphorus removing effect on other harmful substances in sewage, the functions are single, meanwhile, the manufacturing cost is high, the manufacturing method and the process are complex, and the difficulty of batch preparation is improved.
Disclosure of Invention
The invention aims to provide an efficient composite phosphorus removing agent and a preparation method thereof, and aims to solve the problems in the background art.
In order to achieve the purpose, the invention provides the following technical scheme: an efficient composite phosphorus removing agent comprises the following components in percentage by weight: aggregate, biological material, polyferric chloride, polyaluminium chloride, hydrochloric acid, diatomite and deionized water, wherein the weight parts of the components are as follows: 3-10 parts of aggregate, 10-20 parts of biomass, 10-15 parts of polyferric chloride, 10-15 parts of polyaluminium chloride, 50-80 parts of hydrochloric acid, 15-20 parts of diatomite and 10-20 parts of deionized water.
Preferably, the aggregate is prepared by mixing shells, pig bones and cow bones according to the proportion of 3: 1.
Preferably, the biological material is formed by mixing coconut shells, straws and dead wood according to the proportion of 1: 1.
Preferably, the concentration of the hydrochloric acid is 35-37%.
A preparation method of a high-efficiency composite phosphorus removing agent comprises the following steps of firstly, weighing raw materials; crushing the aggregate; step three, dissolving and extracting; step four, mixing and emulsifying; step five, drying at high temperature; step six, carbonizing the biological material; step seven, crushing and mixing; step eight, ultrasonic treatment; step nine, drying and packaging;
in the first step, 3-10 parts of aggregate, 10-20 parts of raw materials, 10-15 parts of polyferric chloride, 10-15 parts of polyaluminium chloride, 50-80 parts of hydrochloric acid, 15-20 parts of kieselguhr and 10-20 parts of deionized water are weighed according to the parts by weight of the components;
in the second step, the aggregate weighed in the first step is taken, washed, dried and ground into powder by a grinder for later use;
adding the bone meal prepared in the step two into a glass container in the step three, then adding the hydrochloric acid weighed in the step one, stirring for full reaction, heating a beaker after the reaction is finished, volatilizing redundant hydrochloric acid to prepare a liquid mixture for later use;
in the fourth step, the liquid mixture prepared in the third step is added into a high-shear emulsifying machine, and then the diatomite weighed in the first step and deionized water are added for full emulsification and shearing to prepare an emulsified mixture for later use;
in the fifth step, the emulsified mixture prepared in the fourth step is put into a high-temperature drying oven at the temperature of 180 ℃ and 200 ℃ for drying for 5-10h to prepare a solid mixture for later use;
in the sixth step, the biological material weighed in the first step is taken and placed into a muffle furnace for preheating, nitrogen is introduced after preheating is finished, and high-temperature carbonization is carried out under the protection of nitrogen to prepare a carbonized material for later use;
adding the solid mixture prepared in the step five and the carbonized material prepared in the step six into a ball mill for ball milling and mixing, adding the polyaluminium chloride and the polyferric chloride weighed in the step one during mixing, and preparing a semi-finished product of the composite phosphorus removing agent for later use after mixing;
in the eighth step, the composite phosphorus removing agent semi-finished product prepared in the seventh step is subjected to ultrasonic mixing by using an ultrasonic generator, and is ready for use after completion;
and in the ninth step, drying the semi-finished product of the composite phosphorus removing agent subjected to the ultrasonic treatment in the eighth step again by using a dryer, cooling to room temperature after drying to prepare a finished product of the composite phosphorus removing agent, and weighing and packaging the finished product of the composite phosphorus removing agent to complete the preparation of the composite phosphorus removing agent.
Preferably, in the third step, the reaction time is 60-120 min.
Preferably, in the fourth step, the rotation speed of the high-shear emulsifying machine is 3500-.
Preferably, in the sixth step, the preheating temperature is 200-300 ℃, the preheating time is 2-3h, the high-temperature carbonization temperature is 800-1500 ℃, and the high-temperature carbonization time is 3-5 h.
Preferably, in the ninth step, the drying temperature is 100-110 ℃, and the drying time is 10-20 h.
Compared with the prior art, the invention has the beneficial effects that:
1. according to the invention, the carbonized material prepared from coconut shells, straws and dead wood is added into the composite phosphorus removing agent, the carbonized material has rich pores and large specific surface area, the adsorption effect of the composite phosphorus removing agent is improved, other harmful substances are removed while phosphorus is removed, and the functional diversity of the composite phosphorus removing agent is improved;
2. according to the invention, hydrochloric acid is used for extracting calcium ions in shells, pig bones and cattle bones to obtain soluble calcium ions, the calcium ions are easy to synthesize insoluble substances with phosphorus elements, so that the effect of phosphorus removal is achieved, and the effect and efficiency of phosphorus removal of the composite phosphorus removing agent are greatly enhanced by matching with the use of polymeric ferric chloride and polymeric aluminum;
3. the preparation method is simple, the raw materials are easy to obtain, waste materials are changed into valuable materials, the waste materials are utilized, the production cost is reduced, the economic benefit is improved, and the environment is protected.
Drawings
FIG. 1 is a flow chart of the method of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1, a technical solution provided by the present invention:
example 1:
an efficient composite phosphorus removing agent comprises the following components in percentage by weight: aggregate, biological material, polyferric chloride, polyaluminium chloride, hydrochloric acid, diatomite and deionized water, wherein the weight parts of the components are as follows: the raw materials comprise 3 parts of aggregate, 10 parts of raw materials, 10 parts of polyferric chloride, 10 parts of polyaluminium chloride, 50 parts of hydrochloric acid, 15 parts of diatomite and 10 parts of deionized water, wherein the aggregate is formed by mixing shells, pig bones and ox bones according to the ratio of 3: 1, the raw materials are formed by mixing coconut shells, straws and cumwood according to the ratio of 1: 1, and the concentration of the hydrochloric acid is 37%.
A preparation method of a high-efficiency composite phosphorus removing agent comprises the following steps of firstly, weighing raw materials; crushing the aggregate; step three, dissolving and extracting; step four, mixing and emulsifying; step five, drying at high temperature; step six, carbonizing the biological material; step seven, crushing and mixing; step eight, ultrasonic treatment; step nine, drying and packaging;
in the first step, 3 parts of aggregate, 10 parts of raw material, 10 parts of polyferric chloride, 10 parts of polyaluminium chloride, 50 parts of hydrochloric acid, 15 parts of diatomite and 10 parts of deionized water are weighed according to the parts by weight of the components;
in the second step, the aggregate weighed in the first step is taken, washed, dried and ground into powder by a grinder for later use;
adding the bone meal prepared in the step two into a glass container in the step three, then adding the hydrochloric acid weighed in the step one, stirring for sufficient reaction for 120min, heating a beaker after the reaction is finished, volatilizing redundant hydrochloric acid to prepare a liquid mixture for later use;
in the fourth step, the liquid mixture prepared in the third step is added into a high-shear emulsifying machine, then the diatomite weighed in the first step and deionized water are added for full emulsification and shearing, the rotating speed of the high-shear emulsifying machine is 3500r/min, the emulsification and shearing time is 15min, and an emulsified mixture is prepared for later use;
in the fifth step, the emulsified mixture prepared in the fourth step is put into a high-temperature drying oven at 180 ℃ for drying for 7 hours to prepare a solid mixture for later use;
in the sixth step, the biological material weighed in the first step is taken and placed into a muffle furnace for preheating, nitrogen is introduced after preheating is finished, high-temperature carbonization is carried out under the protection of nitrogen, the preheating temperature is 300 ℃, the preheating time is 3 hours, the high-temperature carbonization temperature is 900 ℃, the high-temperature carbonization time is 5 hours, and the carbonized material is prepared for later use;
adding the solid mixture prepared in the step five and the carbonized material prepared in the step six into a ball mill for ball milling and mixing, adding the polyaluminium chloride and the polyferric chloride weighed in the step one during mixing, and preparing a semi-finished product of the composite phosphorus removing agent for later use after mixing;
in the eighth step, the composite phosphorus removing agent semi-finished product prepared in the seventh step is subjected to ultrasonic mixing by using an ultrasonic generator, and is ready for use after completion;
and in the ninth step, drying the semi-finished product of the composite phosphorus removing agent subjected to the ultrasonic treatment in the eighth step again by using a dryer, wherein the drying temperature is 110 ℃, the drying time is 15 hours, cooling to room temperature after the drying is finished to prepare a finished product of the composite phosphorus removing agent, and weighing and packaging the finished product of the composite phosphorus removing agent to finish the preparation of the composite phosphorus removing agent.
Example 2:
an efficient composite phosphorus removing agent comprises the following components in percentage by weight: aggregate, biological material, polyferric chloride, polyaluminium chloride, hydrochloric acid, diatomite and deionized water, wherein the weight parts of the components are as follows: 8 parts of aggregate, 15 parts of raw material, 12 parts of polyferric chloride, 12 parts of polyaluminium chloride, 60 parts of hydrochloric acid, 18 parts of diatomite and 15 parts of deionized water, wherein the aggregate is formed by mixing shells, pig bones and ox bones according to the ratio of 3: 1, the raw material is formed by mixing coconut shells, straws and cumwood according to the ratio of 1: 1, and the concentration of the hydrochloric acid is 37%.
A preparation method of a high-efficiency composite phosphorus removing agent comprises the following steps of firstly, weighing raw materials; crushing the aggregate; step three, dissolving and extracting; step four, mixing and emulsifying; step five, drying at high temperature; step six, carbonizing the biological material; step seven, crushing and mixing; step eight, ultrasonic treatment; step nine, drying and packaging;
in the first step, 8 parts of aggregate, 15 parts of raw material, 12 parts of polyferric chloride, 12 parts of polyaluminium chloride, 60 parts of hydrochloric acid, 18 parts of diatomite and 15 parts of deionized water are weighed according to the parts by weight of the components;
in the second step, the aggregate weighed in the first step is taken, cleaned and dried, and then ground into powder by a grinder for later use;
adding the bone meal prepared in the step two into a glass container in the step three, then adding the hydrochloric acid weighed in the step one, stirring for sufficient reaction for 120min, heating a beaker after the reaction is finished, volatilizing redundant hydrochloric acid to prepare a liquid mixture for later use;
in the fourth step, the liquid mixture prepared in the third step is added into a high-shear emulsifying machine, then the diatomite weighed in the first step and deionized water are added for full emulsification and shearing, the rotating speed of the high-shear emulsifying machine is 3500r/min, the emulsification and shearing time is 15min, and an emulsified mixture is prepared for later use;
in the fifth step, the emulsified mixture prepared in the fourth step is put into a high-temperature drying oven at 180 ℃ for drying for 7 hours to prepare a solid mixture for later use;
in the sixth step, the biological material weighed in the first step is taken and placed into a muffle furnace for preheating, nitrogen is introduced after preheating is finished, high-temperature carbonization is carried out under the protection of nitrogen, the preheating temperature is 300 ℃, the preheating time is 3 hours, the high-temperature carbonization temperature is 900 ℃, the high-temperature carbonization time is 5 hours, and the carbonized material is prepared for later use;
adding the solid mixture prepared in the step five and the carbonized material prepared in the step six into a ball mill for ball milling and mixing, adding the polyaluminium chloride and the polyferric chloride weighed in the step one during mixing, and preparing a semi-finished product of the composite phosphorus removing agent for later use after mixing;
in the eighth step, the composite phosphorus removing agent semi-finished product prepared in the seventh step is subjected to ultrasonic mixing by using an ultrasonic generator, and is ready for use after completion;
and in the ninth step, drying the semi-finished product of the composite phosphorus removing agent subjected to the ultrasonic treatment in the eighth step again by using a dryer, wherein the drying temperature is 110 ℃, the drying time is 15 hours, cooling to room temperature after the drying is finished to prepare a finished product of the composite phosphorus removing agent, and weighing and packaging the finished product of the composite phosphorus removing agent to finish the preparation of the composite phosphorus removing agent.
Example 3:
an efficient composite phosphorus removing agent comprises the following components in percentage by weight: aggregate, biological material, polyferric chloride, polyaluminium chloride, hydrochloric acid, diatomite and deionized water, wherein the weight parts of the components are as follows: 10 parts of aggregate, 20 parts of raw material, 15 parts of polyferric chloride, 15 parts of polyaluminium chloride, 80 parts of hydrochloric acid, 20 parts of diatomite and 20 parts of deionized water, wherein the aggregate is formed by mixing shells, pig bones and ox bones according to the ratio of 3: 1, the raw material is formed by mixing coconut shells, straws and cumwood according to the ratio of 1: 1, and the concentration of the hydrochloric acid is 37%.
A preparation method of a high-efficiency composite phosphorus removing agent comprises the following steps of firstly, weighing raw materials; crushing the aggregate; step three, dissolving and extracting; step four, mixing and emulsifying; step five, drying at high temperature; step six, carbonizing the biological material; step seven, crushing and mixing; step eight, ultrasonic treatment; step nine, drying and packaging;
in the first step, respectively weighing 10 parts of aggregate, 20 parts of raw material, 15 parts of polyferric chloride, 15 parts of polyaluminium chloride, 80 parts of hydrochloric acid, 20 parts of diatomite and 20 parts of deionized water according to the parts by weight of the components;
in the second step, the aggregate weighed in the first step is taken, washed, dried and ground into powder by a grinder for later use;
adding the bone meal prepared in the step two into a glass container in the step three, then adding the hydrochloric acid weighed in the step one, stirring for sufficient reaction for 120min, heating a beaker after the reaction is finished, volatilizing redundant hydrochloric acid to prepare a liquid mixture for later use;
in the fourth step, the liquid mixture prepared in the third step is added into a high-shear emulsifying machine, then the diatomite weighed in the first step and deionized water are added for full emulsification and shearing, the rotating speed of the high-shear emulsifying machine is 3500r/min, the emulsification and shearing time is 15min, and an emulsified mixture is prepared for later use;
in the fifth step, the emulsified mixture prepared in the fourth step is put into a high-temperature drying oven at 180 ℃ for drying for 7 hours to prepare a solid mixture for later use;
in the sixth step, the biological material weighed in the first step is taken and placed into a muffle furnace for preheating, nitrogen is introduced after preheating is finished, high-temperature carbonization is carried out under the protection of nitrogen, the preheating temperature is 300 ℃, the preheating time is 3 hours, the high-temperature carbonization temperature is 900 ℃, the high-temperature carbonization time is 5 hours, and the carbonized material is prepared for later use;
adding the solid mixture prepared in the step five and the carbonized material prepared in the step six into a ball mill for ball milling and mixing, adding the polyaluminium chloride and the polyferric chloride weighed in the step one during mixing, and preparing a semi-finished product of the composite phosphorus removing agent for later use after mixing;
in the eighth step, the composite phosphorus removing agent semi-finished product prepared in the seventh step is subjected to ultrasonic mixing by using an ultrasonic generator, and is ready for use after completion;
and in the ninth step, drying the semi-finished product of the composite phosphorus removing agent subjected to the ultrasonic treatment in the eighth step again by using a dryer, wherein the drying temperature is 110 ℃, the drying time is 15 hours, cooling to room temperature after the drying is finished to prepare a finished product of the composite phosphorus removing agent, and weighing and packaging the finished product of the composite phosphorus removing agent to finish the preparation of the composite phosphorus removing agent.
The properties of the examples are compared in the following table:
Figure BDA0003497073400000081
Figure BDA0003497073400000091
based on the above, the invention uses the carbonized material prepared by high-temperature carbonization of coconut shells, straws and dead wood as the raw material to prepare the composite phosphorus removal agent, the carbonized material has a large number of pores and large specific surface area, which is beneficial to improving the adsorption capacity of the composite phosphorus removal agent, has the same removing effect on other harmful substances in sewage while removing phosphorus, improves the functional diversity of the composite phosphorus removal agent, simultaneously utilizes hydrochloric acid to extract calcium ions in a free state after grinding shells, pig bones and cattle bones, and then is added into the composite phosphorus removal agent as the raw material, the calcium ions and the phosphorus are easy to combine to generate water-insoluble substances, thereby achieving the phosphorus removal effect, and the phosphorus removal efficiency and the effect of the composite phosphorus removal agent are greatly increased by matching with the phosphorus removal effect of polymeric ferric chloride and polymeric aluminum chloride, the invention uses the waste coconut shells, straws, dead wood, shells, pig bones and cattle bones to prepare the composite phosphorus removal agent, realizes the utilization of waste, is beneficial to environmental protection and reduces the production cost at the same time.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.

Claims (9)

1. An efficient composite phosphorus removing agent comprises the following components in percentage by weight: aggregate, biological material, polymeric ferric chloride, polyaluminium chloride, hydrochloric acid, diatomite and deionized water, and is characterized in that: the weight parts of each component are respectively as follows: 3-10 parts of aggregate, 10-20 parts of biomass, 10-15 parts of polyferric chloride, 10-15 parts of polyaluminium chloride, 50-80 parts of hydrochloric acid, 15-20 parts of diatomite and 10-20 parts of deionized water.
2. The efficient composite phosphorus removing agent as claimed in claim 1, wherein: the aggregate is prepared by mixing shells, pig bones and cow bones according to the proportion of 3: 1.
3. The efficient composite phosphorus removing agent as claimed in claim 1, wherein: the biological material is formed by mixing coconut shells, straws and dead wood according to the proportion of 1: 1.
4. The efficient composite phosphorus removing agent as claimed in claim 1, wherein: the concentration of the hydrochloric acid is 35-37%.
5. A preparation method of a high-efficiency composite phosphorus removing agent comprises the following steps of firstly, weighing raw materials; crushing the aggregate; step three, dissolving and extracting; step four, mixing and emulsifying; step five, drying at high temperature; step six, carbonizing the biological material; step seven, crushing and mixing; step eight, ultrasonic treatment; step nine, drying and packaging; the method is characterized in that:
in the first step, 3-10 parts of aggregate, 10-20 parts of raw materials, 10-15 parts of polyferric chloride, 10-15 parts of polyaluminium chloride, 50-80 parts of hydrochloric acid, 15-20 parts of kieselguhr and 10-20 parts of deionized water are weighed according to the parts by weight of the components;
in the second step, the aggregate weighed in the first step is taken, washed, dried and ground into powder by a grinder for later use;
adding the bone meal prepared in the step two into a glass container in the step three, then adding the hydrochloric acid weighed in the step one, stirring for full reaction, heating a beaker after the reaction is finished, volatilizing redundant hydrochloric acid to prepare a liquid mixture for later use;
in the fourth step, the liquid mixture prepared in the third step is added into a high-shear emulsifying machine, and then the diatomite weighed in the first step and deionized water are added for full emulsification and shearing to prepare an emulsified mixture for later use;
wherein in the fifth step, the emulsified mixture prepared in the fourth step is put into a high-temperature drying oven with the temperature of 180 ℃ and 200 ℃ for drying for 5-10h to prepare a solid mixture for standby;
in the sixth step, the biological material weighed in the first step is taken and placed into a muffle furnace for preheating, nitrogen is introduced after preheating is finished, and high-temperature carbonization is carried out under the protection of nitrogen to prepare a carbonized material for later use;
adding the solid mixture prepared in the step five and the carbonized material prepared in the step six into a ball mill for ball milling and mixing, adding the polyaluminium chloride and the polyferric chloride weighed in the step one during mixing, and preparing a semi-finished product of the composite phosphorus removing agent for later use after mixing;
in the eighth step, the composite phosphorus removing agent semi-finished product prepared in the seventh step is subjected to ultrasonic mixing by using an ultrasonic generator, and is ready for use after completion;
and in the ninth step, drying the semi-finished product of the composite phosphorus removing agent subjected to the ultrasonic treatment in the eighth step again by using a dryer, cooling to room temperature after drying to prepare a finished product of the composite phosphorus removing agent, and weighing and packaging the finished product of the composite phosphorus removing agent to complete the preparation of the composite phosphorus removing agent.
6. The preparation method of the efficient composite phosphorus removing agent as claimed in claim 5, characterized in that: in the third step, the reaction time is 60-120 min.
7. The preparation method of the efficient composite phosphorus removal agent as claimed in claim 5, wherein: in the fourth step, the rotating speed of the high-shear emulsifying machine is 3500-5000r/min, and the emulsifying and shearing time is 10-15 min.
8. The preparation method of the efficient composite phosphorus removal agent as claimed in claim 5, wherein: in the sixth step, the preheating temperature is 200-300 ℃, the preheating time is 2-3h, the high-temperature carbonization temperature is 800-1500 ℃, and the high-temperature carbonization time is 3-5 h.
9. The preparation method of the efficient composite phosphorus removal agent as claimed in claim 5, wherein: in the ninth step, the drying temperature is 100-.
CN202210117530.9A 2022-02-08 2022-02-08 Efficient composite phosphorus removal agent and preparation method thereof Pending CN114471462A (en)

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Publication number Priority date Publication date Assignee Title
CN104291420A (en) * 2014-09-11 2015-01-21 陕西省石油化工研究设计院 Phosphorus removing agent containing inorganic mineral and application method thereof
CN106187798A (en) * 2016-07-21 2016-12-07 西安利君制药有限责任公司 A kind of chelated calcium preparation method of aminoacid nanometer
CN106975455A (en) * 2017-05-08 2017-07-25 宁波市川宁环保科技有限公司 A kind of calcium matrix activated carbon absorption phosphor-curing agent and preparation method thereof
CN109908865A (en) * 2019-03-25 2019-06-21 武汉理工大学 A kind of preparation method and applications of pig bone and bamboo wood copyrolysis charcoal
CN112705165A (en) * 2021-01-05 2021-04-27 中国科学院青岛生物能源与过程研究所 Preparation method and application of shell-straw-based calcium-rich biochar

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104291420A (en) * 2014-09-11 2015-01-21 陕西省石油化工研究设计院 Phosphorus removing agent containing inorganic mineral and application method thereof
CN106187798A (en) * 2016-07-21 2016-12-07 西安利君制药有限责任公司 A kind of chelated calcium preparation method of aminoacid nanometer
CN106975455A (en) * 2017-05-08 2017-07-25 宁波市川宁环保科技有限公司 A kind of calcium matrix activated carbon absorption phosphor-curing agent and preparation method thereof
CN109908865A (en) * 2019-03-25 2019-06-21 武汉理工大学 A kind of preparation method and applications of pig bone and bamboo wood copyrolysis charcoal
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