CN113244877A - Formula and preparation method of nitrogen-doped hydroxyl copper phosphate adsorbent - Google Patents

Formula and preparation method of nitrogen-doped hydroxyl copper phosphate adsorbent Download PDF

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Publication number
CN113244877A
CN113244877A CN202110642010.5A CN202110642010A CN113244877A CN 113244877 A CN113244877 A CN 113244877A CN 202110642010 A CN202110642010 A CN 202110642010A CN 113244877 A CN113244877 A CN 113244877A
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China
Prior art keywords
mass
nitrogen
copper
phosphoric acid
raw materials
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CN202110642010.5A
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Chinese (zh)
Inventor
赵德强
余玲
刘海楠
黄琦
黎琪
王胜
张倩
张冰瑶
赵正刚
宋南川
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Chongqing Jiaotong University
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Chongqing Jiaotong University
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Priority to CN202110642010.5A priority Critical patent/CN113244877A/en
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • 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
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/0203—Solid 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
    • B01J20/0274—Solid 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
    • B01J20/0292—Phosphates of compounds other than those provided for in B01J20/048
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • 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
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/0203—Solid 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
    • B01J20/0233—Compounds of Cu, Ag, Au
    • B01J20/0237—Compounds of Cu
    • C—CHEMISTRY; METALLURGY
    • 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
    • C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Analytical Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Hydrology & Water Resources (AREA)
  • Water Supply & Treatment (AREA)
  • Environmental & Geological Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)

Abstract

The invention discloses a formula and a preparation method of a nitrogen-doped hydroxyl copper phosphate adsorbent, and relates to the technical field of atmospheric treatment and water treatment. The formula of the invention comprises the following raw materials in parts by weight: the phosphoric acid, copper acetate with the mass being 70-80% of the mass of the phosphoric acid, ethylenediamine with the mass being 5-15% of the mass of the phosphoric acid, phosphate with the mass being 50-70% of the mass of the phosphoric acid, soluble copper salt with the mass being 80-130% of the mass of the phosphoric acid and nitrogen with the mass being 3-10% of the mass of the phosphoric acid. The invention has the advantages of easily obtained materials, low price and simpler production process, and the produced adsorbent can effectively adsorb pollutants in the atmosphere and water, can better purify the pollutants in the atmosphere and water, and is suitable for large-scale popularization.

Description

Formula and preparation method of nitrogen-doped hydroxyl copper phosphate adsorbent
Technical Field
The invention belongs to the technical field of atmospheric treatment and water treatment, and particularly relates to a formula and a preparation method of a nitrogen-doped hydroxyl copper phosphate adsorbent.
Background
The atmosphere is the air surrounding the earth, and the influence of atmospheric pollution on the physical state of the atmosphere mainly causes the abnormal change of climate;
the water is an inorganic substance consisting of two elements of hydrogen and oxygen, is non-toxic, is colorless and odorless transparent liquid at normal temperature and normal pressure, is called as a source of human life, is one of the most common substances on the earth, is an important resource for all lives including inorganic compounds and human beings, is also the most important component of organisms, plays an important role in life evolution, and water pollution refers to the pollution of water bodies by pollutants;
the polluted atmosphere and water can cause great influence on the ecological environment, so that the living environment of human beings is greatly influenced, and therefore, the pollutants in the atmosphere and the water need to be purified;
however, when the prior art is used for purifying pollutants in the atmosphere and water, the purification effect is poor, the raw materials are rare, the price is high, the production cost is high, the production process is complex, and the method is not suitable for large-scale popularization.
Disclosure of Invention
The invention aims to provide a formula and a preparation method of a nitrogen-doped hydroxyl copper phosphate adsorbent, which aim to solve the existing problems: when the prior art is used for purifying pollutants in the atmosphere and water, the purification effect is poor, the raw materials are rare, the price is high, the production cost is high, the production process is complex, and the method is not suitable for large-scale popularization.
In order to solve the technical problems, the invention is realized by the following technical scheme:
the invention relates to a formula of a nitrogen-doped hydroxyl copper phosphate adsorbent, which comprises the following raw materials in parts by weight:
the phosphoric acid, copper acetate with the mass being 70-80% of the mass of the phosphoric acid, ethylenediamine with the mass being 5-15% of the mass of the phosphoric acid, phosphate with the mass being 50-70% of the mass of the phosphoric acid, soluble copper salt with the mass being 80-130% of the mass of the phosphoric acid and nitrogen with the mass being 3-10% of the mass of the phosphoric acid.
Further, the phosphate is one of ammonium phosphate, sodium phosphate and potassium phosphate.
Further, the soluble copper salt is selected from one of copper nitrate, copper chloride and copper sulfate.
Further, the formula comprises the following raw materials in parts by weight:
phosphoric acid, 74% by mass of copper acetate, 12% by mass of ethylenediamine, 65% by mass of phosphate, 100% by mass of soluble copper salt and 5% by mass of nitrogen.
A method for preparing a nitrogen-doped copper hydroxyphosphate adsorbent for use in any one of the above nitrogen-doped copper hydroxyphosphate adsorbent formulations, said method comprising the steps of:
heating the raw material to heat the raw material and water;
the raw materials are phosphoric acid, copper acetate, ethylenediamine, phosphate and soluble copper salt;
stirring the raw materials, namely stirring the raw materials and water;
washing the raw materials, namely washing the raw materials by adopting deionized water and ethanol alternately;
filtering the raw material to filter the raw material;
drying the raw materials, calcining the raw materials, and adding nitrogen;
and grinding the raw materials, wherein the raw materials are ground.
Further, the heating temperature of the raw material is 180-240 ℃, and the heating time is 2-6 hours.
Further, the stirring time is 0.5-1 h.
Further, the calcining temperature is 240-350 ℃, and the calcining time is 2-2.5 h.
Further, the particle size of the ground raw materials is 0.5-20.0 microns.
The invention has the following beneficial effects:
the invention has the advantages of easily obtained materials, low price and simpler production process, and the produced adsorbent can effectively adsorb pollutants in the atmosphere and water, can better purify the pollutants in the atmosphere and water, and is suitable for large-scale popularization.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all 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.
The first embodiment is as follows:
the invention relates to a formula of a nitrogen-doped hydroxyl copper phosphate adsorbent, which comprises the following raw materials in parts by weight:
phosphoric acid, copper acetate accounting for 70 percent of the mass of the phosphoric acid, ethylenediamine accounting for 5 percent of the mass of the phosphoric acid, phosphate accounting for 50 percent of the mass of the phosphoric acid, soluble copper salt accounting for 80 percent of the mass of the phosphoric acid and nitrogen accounting for 3 percent of the mass of the phosphoric acid;
wherein the phosphate is one of ammonium phosphate, sodium phosphate and potassium phosphate;
and the soluble copper salt is selected from one of copper nitrate, copper chloride and copper sulfate.
Example two:
the formula comprises the following raw materials in parts by weight:
phosphoric acid, 74% by mass of copper acetate, 12% by mass of ethylenediamine, 65% by mass of phosphate, 100% by mass of soluble copper salt and 5% by mass of nitrogen.
Example three:
the formula comprises the following raw materials in parts by weight:
phosphoric acid, 80% by mass of copper acetate, 15% by mass of ethylenediamine, 70% by mass of phosphate, 130% by mass of a soluble copper salt and 10% by mass of nitrogen.
Example four:
on the basis of the first embodiment, the second embodiment or the third embodiment, the preparation method of the nitrogen-doped copper hydroxyphosphate adsorbent is disclosed, and the preparation method comprises the following steps:
heating the raw material to heat the raw material and water;
the raw materials are phosphoric acid, copper acetate, ethylenediamine, phosphate and soluble copper salt
The heating temperature of the raw material is 180-240 ℃, and the heating time is 2-6 hours;
stirring the raw materials, namely stirring the raw materials and water for 0.5-1 h;
washing the raw materials, namely washing the raw materials by adopting deionized water and ethanol alternately until the raw materials are washed to be neutral;
filtering the raw material to filter the raw material;
drying the raw materials, calcining the raw materials, and adding nitrogen;
the calcining temperature is 240-350 ℃, and the calcining time is 2-2.5 h;
grinding the raw materials until the particle size of the raw materials is 0.5-20.0 microns;
in conclusion, the invention has the advantages of easily available materials, low price and simpler production process, the produced adsorbent can effectively adsorb pollutants in the atmosphere and water, such as metal and carbon dioxide, can better purify the pollutants in the atmosphere and water, and is suitable for large-scale popularization.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise embodiments disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention. The invention is limited only by the claims and their full scope and equivalents.

Claims (9)

1. The formula of the nitrogen-doped hydroxyl copper phosphate adsorbent is characterized by comprising the following raw materials in parts by weight:
the phosphoric acid, copper acetate with the mass being 70-80% of the mass of the phosphoric acid, ethylenediamine with the mass being 5-15% of the mass of the phosphoric acid, phosphate with the mass being 50-70% of the mass of the phosphoric acid, soluble copper salt with the mass being 80-130% of the mass of the phosphoric acid and nitrogen with the mass being 3-10% of the mass of the phosphoric acid.
2. The nitrogen-doped copper hydroxyphosphate adsorbent formulation according to claim 1, wherein the phosphate is one of ammonium phosphate, sodium phosphate and potassium phosphate.
3. The adsorbent formulation of claim 1, wherein the soluble copper salt is selected from the group consisting of copper nitrate, copper chloride, and copper sulfate.
4. The formula of the nitrogen-doped copper hydroxyphosphate adsorbent according to claim 1, wherein the formula comprises the following raw materials in parts by weight:
phosphoric acid, 74% by mass of copper acetate, 12% by mass of ethylenediamine, 65% by mass of phosphate, 100% by mass of soluble copper salt and 5% by mass of nitrogen.
5. A method of preparing a nitrogen-doped copper hydroxyphosphate adsorbent for use in a nitrogen-doped copper hydroxyphosphate adsorbent formulation according to any one of claims 1 to 4, comprising the steps of:
heating the raw material to heat the raw material and water;
the raw materials are phosphoric acid, copper acetate, ethylenediamine, phosphate and soluble copper salt;
stirring the raw materials, namely stirring the raw materials and water;
washing the raw materials, namely washing the raw materials by adopting deionized water and ethanol alternately;
filtering the raw material to filter the raw material;
drying the raw materials, calcining the raw materials, and adding nitrogen;
and grinding the raw materials, wherein the raw materials are ground.
6. The formula and the preparation method of the nitrogen-doped copper hydroxyphosphate adsorbent according to claim 5, wherein the raw material is heated at 180-240 ℃ for 2-6 h.
7. The formula and the preparation method of the nitrogen-doped copper hydroxyphosphate according to claim 5, wherein the stirring time is 0.5-1 h.
8. The formula and the preparation method of the nitrogen-doped copper hydroxyphosphate according to claim 5, wherein the calcination temperature is 240-350 ℃, and the calcination time is 2-2.5 h.
9. The formula and the preparation method of the nitrogen-doped copper hydroxyphosphate adsorbent according to claim 5, wherein the particle size of the raw material after grinding is 0.5-20.0 microns.
CN202110642010.5A 2021-06-09 2021-06-09 Formula and preparation method of nitrogen-doped hydroxyl copper phosphate adsorbent Pending CN113244877A (en)

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Citations (7)

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Publication number Priority date Publication date Assignee Title
CN103803539A (en) * 2014-02-17 2014-05-21 上海交通大学 Nitrogen-doped graphene oxide material and preparation method thereof
WO2014162255A1 (en) * 2013-04-01 2014-10-09 Sabic Innovative Plastics Ip B.V. High modulus laser direct structuring polycarbonate composites with enhanced plating performance and broad laser window and methods for the manufacture and use thereof
CN105309427A (en) * 2015-12-03 2016-02-10 日正九安科技（北京）有限公司 Copper ethylenediamine bactericide composition and preparation method thereof
CN106984267A (en) * 2017-03-23 2017-07-28 青岛科技大学 A kind of preparation method of the N doping carbon adsorbent of CO absorption 2
CN107899537A (en) * 2017-11-29 2018-04-13 长沙埃比林环保科技有限公司 A kind of alkali formula cupric phosphate sorbing material and preparation method thereof
CN111377443A (en) * 2018-12-29 2020-07-07 中国石油化工股份有限公司 Copper-doped activated carbon composite material and preparation method thereof
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Publication number Priority date Publication date Assignee Title
WO2014162255A1 (en) * 2013-04-01 2014-10-09 Sabic Innovative Plastics Ip B.V. High modulus laser direct structuring polycarbonate composites with enhanced plating performance and broad laser window and methods for the manufacture and use thereof
CN103803539A (en) * 2014-02-17 2014-05-21 上海交通大学 Nitrogen-doped graphene oxide material and preparation method thereof
CN105309427A (en) * 2015-12-03 2016-02-10 日正九安科技（北京）有限公司 Copper ethylenediamine bactericide composition and preparation method thereof
CN106984267A (en) * 2017-03-23 2017-07-28 青岛科技大学 A kind of preparation method of the N doping carbon adsorbent of CO absorption 2
CN107899537A (en) * 2017-11-29 2018-04-13 长沙埃比林环保科技有限公司 A kind of alkali formula cupric phosphate sorbing material and preparation method thereof
CN111377443A (en) * 2018-12-29 2020-07-07 中国石油化工股份有限公司 Copper-doped activated carbon composite material and preparation method thereof
CN111992201A (en) * 2020-08-21 2020-11-27 重庆交通大学 One-step synthesis of BiVO by microwave hydrothermal method4/InVO4Method and application of photocatalyst

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Application publication date: 20210813