CN109174044B - Method for improving specific surface area and adsorption capacity of opal - Google Patents

Method for improving specific surface area and adsorption capacity of opal Download PDF

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CN109174044B
CN109174044B CN201811003092.3A CN201811003092A CN109174044B CN 109174044 B CN109174044 B CN 109174044B CN 201811003092 A CN201811003092 A CN 201811003092A CN 109174044 B CN109174044 B CN 109174044B
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opal
powder
alkali source
surface area
specific surface
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CN109174044A (en
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任子杰
卞政
高惠民
张安岭
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Shanxi Zhihui Chuangxin technology material Co.,Ltd.
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Wuhan University of Technology WUT
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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
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
    • B01J20/28057—Surface area, e.g. B.E.T specific surface area
    • 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
    • B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/16—Alumino-silicates
    • B01J20/165—Natural alumino-silicates, e.g. zeolites
    • 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
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
    • B01J20/28057—Surface area, e.g. B.E.T specific surface area
    • B01J20/28059—Surface area, e.g. B.E.T specific surface area being less than 100 m2/g
    • 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
    • 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
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/30—Organic compounds
    • C02F2101/36—Organic compounds containing halogen
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/30—Organic compounds
    • C02F2101/38—Organic compounds containing nitrogen
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/30—Organic compounds
    • C02F2101/40—Organic compounds containing sulfur

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

Abstract

The invention relates to a method for improving the specific surface area and the adsorption capacity of opal, which uses natural or roasted opal, an alkali source and MgCl2The glycerol is used as a raw material, the glycerol is subjected to aerobic steam pressure treatment after being uniformly mixed, zeolite phase is generated on the surface of the protein soil shell, so that the adsorbability of the protein soil shell is enhanced, meanwhile, the microporous structure on the surface of the protein soil is more complex and diversified, the specific surface area of the protein soil is also remarkably increased in the process, and the adsorption capacity is further improved. The method greatly improves the application effect and value of the opal in the fields of adsorbents, filter aids and the like.

Description

Method for improving specific surface area and adsorption capacity of opal
Technical Field
The invention relates to the technical field of nonmetallic mineral processing and environmental engineering, in particular to a method for improving the specific surface area and the adsorption capacity of opal.
Background
The opal is aqueous amorphous active silicon dioxide, the main chemical composition of which is SiO2、AlO3、Fe2O3、TiO2And also contains small amount of MgO, CaO and organic matter. The protein soil has the advantages of light weight, high porosity, strong water absorption and the like. The protein soil is produced in China as siliceous mineral products with abundant reserves, Henan, Shaanxi, Yunnan, Heilongjiang and the like, and has been widely applied to industrial production, such as filter aids, decolorants, stabilizers of paper pulp bleaching agents, coatings and the like.
Natural opals consist of tiny opal spheres. The single protein soil has pores, so that the single protein soil has strong adsorption capacity, and when the single protein soil is used as a filter aid in industry, the single protein soil is generally subjected to bulking and surface treatment by a roasting method, so that on one hand, part of impurities can be removed, and meanwhile, internal fragments can be bonded into larger particles, so that the resistance of the single protein soil to fluid is reduced, and the filtering performance is improved, however, the treatment usually causes the great reduction and even loss of the specific surface area and the adsorption performance, and the application of the single protein soil is greatly limited.
Disclosure of Invention
The invention aims to overcome the problems of the existing opal processing technology and provides a method for improving the specific surface area and the adsorption capacity of the opal, which comprises the following steps:
(a) uniformly mixing the opal with an alkali source to obtain an opal semi-finished powder;
(b) and uniformly mixing the magnesium salt and the alcohol solvent, adding the half-finished product powder of the opal, uniformly mixing, standing, performing autoclaved treatment, and finally drying and crushing.
According to the scheme, the opal is selected from natural opal powder or roasted opal powder with the silicon dioxide content of more than 70%.
According to the scheme, the alkali source is specifically a substance which is alkaline (pH is more than 7) after being mixed with water, and can be a pure substance or a mixture. Such as one of sodium hydroxide, potassium hydroxide, calcium oxide, or a mixture of several thereof. The particle size of the alkali source is below 30 μm.
According to the scheme, the magnesium salt is magnesium chloride, and the alcohol solvent is glycerol.
According to the scheme, the standing time is 30-75min, and the parameters of the steam pressure treatment are as follows: the temperature is 120-.
According to the scheme, the drying mode is drying in an oven, the temperature of the oven is set to be 80-120 ℃, and the dried material is crushed to the granularity of no more than 74 mu m.
According to the scheme, the mass part ratio of the opal, the alkali source, the magnesium salt and the alcohol solvent is 70-95:2-25:1-3: 1-5.
The invention has the beneficial effects that: the well-developed pore structure of the opal is utilized, an external alkali source is used as a main auxiliary material, and the stable zeolite phase is generated on the surface of the opal by adding an alcoholic solution and Mg2+ in combination with aerobic steam pressure reaction, so that the surface micropore structure is increased, the micropore structure is complex and various, and the specific surface area, the adsorption capacity and the permeability of the opal are greatly improved in the process. Compared with natural opal raw materials, the opal material prepared by the invention has the advantages of less useless impurities, transparent pore passages, more surface microporous structures, large specific surface area, good adsorbability and the like.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
In order to make those skilled in the art fully understand the technical solutions and advantages of the present invention, the following embodiments are further described.
The opal soil used in the invention is natural opal soil from a place in Yangtze city, Jilin province, and roasted opal soil obtained by roasting the natural opal soil at 800 ℃ for 40 min. SiO in opal soil2The content is about 80 percent. The CaO, NaOH, etc. used were analytically pure and ground to a particle size of 30 μm or less before use. Other raw materials are all sold in the common market.
Example 1
(1) Respectively weighing 9g of natural opal soil and 1g of NaOH, and stirring for 30min by using a vortex mixer to uniformly mix the natural opal soil and the NaOH to obtain primary opal soil powder;
(2) 1.9g of MgCl were weighed2Preparing 1L of mixed solution with 2.7g of glycerol, taking 50mL of mixed solution, uniformly mixing the mixed solution with the primary opal powder, adding the mixed solution into a 75mL ceramic crucible according to the solid-liquid mass ratio of 1:5, fully stirring, and placing the mixture into a high-pressure reaction kettle to react for 12 hours at 160 ℃; oxygen is not discharged in the temperature rising process, so that the reaction process is ensured to be in an aerobic environment;
(3) and after the reaction is finished, taking out the opal, cooling to room temperature, filtering, fully drying at 100 ℃, and crushing to below 74 microns by using a powder grinding machine to finally obtain the opal powder with high specific surface area and adsorption performance.
Example 2
This embodiment is substantially the same as embodiment 1 except that: the dosage of the natural opal is 8.5g, and the dosage of NaOH is 1.5 g.
Example 3
This embodiment is substantially the same as embodiment 1 except that: the amount of the natural opal is 9.5g, the amount of the NaOH is changed into CaO, the amount of the natural opal is 0.5g, the autoclave reaction temperature is 180 ℃, and the reaction time is unchanged.
Example 4
This embodiment is substantially the same as embodiment 1 except that: the natural opal is roasted before use and then ground into powder.
Example 5
This embodiment is substantially the same as embodiment 1 except that: the natural opal is roasted before use and then ground into powder, the dosage of the powder is 8.5g, and the dosage of NaOH is 1.5 g.
Example 6
This embodiment is substantially the same as embodiment 1 except that: the natural opal is roasted before use, and then ground into powder, the dosage of which is 9.5g, the dosage of NaOH is changed into CaO, the dosage of which is 0.5g, the autoclave reaction temperature is 180 ℃, and the reaction time is unchanged.
In order to fully understand the performance of the protein soil material prepared by the invention, a methylene blue adsorption experiment is carried out, the adsorption amount and the specific surface area of the methylene blue adsorption experiment are used as product evaluation indexes, the test method is strictly carried out according to JC/T2177-2013 Diatom ooze decorative wall material, and related results are shown in Table 1.
TABLE 1 comparison of Properties of the opal Material and the products of examples 1-6
Figure BDA0001783414670000041
As can be seen from Table 1, the adsorption capacity and specific surface area of the obtained opal powder material to methylene blue are greatly improved compared with those of natural opal and roasted opal; by taking roasting opal as an example, the adsorption capacity of the opal powder material prepared by the embodiment of the invention to methylene blue is nearly 10 times, the specific surface area is 25-80 times, and the improvement effect is very obvious.

Claims (9)

1. A method for improving the specific surface area and the adsorption capacity of the opal is characterized by comprising the following steps:
(a) uniformly mixing the opal with an alkali source to obtain an opal semi-finished powder;
(b) and uniformly mixing the magnesium salt and the alcohol solvent, adding the half-finished product powder of the opal, uniformly mixing, standing, performing autoclaved treatment, and finally drying and crushing.
2. The method of claim 1, wherein: the opal is selected from natural opal powder or roasted opal powder with silicon dioxide content of more than 70%.
3. The method of claim 1, wherein: the alkali source is a substance which is alkaline after being mixed with water, and comprises a pure substance or a mixture.
4. The method of claim 3, wherein: the alkali source is selected from one or more of sodium hydroxide, potassium hydroxide and calcium oxide.
5. The method of claim 3, wherein: the particle size of the alkali source is below 30 μm.
6. The method of claim 1, wherein: the magnesium salt is magnesium chloride, and the alcohol solvent is glycerol.
7. The method of claim 1, wherein: standing for 30-75min, wherein the parameters of the steam pressure treatment are as follows: the temperature is 120-.
8. The method of claim 1, wherein: the drying mode is drying in an oven, the temperature of the oven is set to be 80-120 ℃, and the drying is carried out and then the powder is crushed until the granularity is not more than 74 mu m.
9. The method of claim 1, wherein: the mass part ratio of the opal, the alkali source, the magnesium salt and the alcohol solvent is 70-95:2-25:1-3: 1-5.
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CN111774044B (en) * 2020-06-02 2021-04-09 武汉理工大学 Regeneration method of protein soil adsorbent
CN111747421A (en) * 2020-06-02 2020-10-09 武汉理工大学 Method for improving activity of expanded perlite material
CN111672455A (en) * 2020-06-02 2020-09-18 武汉理工大学 Preparation method of high-activity expanded perlite

Citations (2)

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SU662493A1 (en) * 1975-07-29 1979-05-15 Melkonyan Garegin S Method of obtaining complex raw material for glass-making
JP2006247645A (en) * 2005-02-10 2006-09-21 Natoo Kenkyusho:Kk Modification treatment agent, modification treatment method of heat history silicate and binding shape body modified it

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CN103055828B (en) * 2013-02-05 2014-09-03 武汉理工大学 Diatomite/cellulose inorganic-organic composite filter aid for directly filtering micro-polluted water source as well as preparation method and application of diatomite/cellulose inorganic-organic composite filter aid
CN106268629A (en) * 2016-08-17 2017-01-04 吉林大学 A kind of preparation method and applications of the micro-mesopore molecular sieve diatomite composite material for adsorption process
CN107694540B (en) * 2017-09-27 2019-12-24 沈阳建筑大学 Preparation method of diatom morph-genetic hydrated calcium silicate superfine powder for dye removal
CN108358654B (en) * 2018-01-31 2021-05-18 武汉理工大学 Method for preparing high-activity adsorption ceramsite by using low-grade diatomite

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
SU662493A1 (en) * 1975-07-29 1979-05-15 Melkonyan Garegin S Method of obtaining complex raw material for glass-making
JP2006247645A (en) * 2005-02-10 2006-09-21 Natoo Kenkyusho:Kk Modification treatment agent, modification treatment method of heat history silicate and binding shape body modified it

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