CN106276926B - The production method of modified pressure-variable adsorption silica gel - Google Patents

The production method of modified pressure-variable adsorption silica gel Download PDF

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Publication number
CN106276926B
CN106276926B CN201610662435.1A CN201610662435A CN106276926B CN 106276926 B CN106276926 B CN 106276926B CN 201610662435 A CN201610662435 A CN 201610662435A CN 106276926 B CN106276926 B CN 106276926B
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acid
silica gel
production method
variable adsorption
modified pressure
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CN106276926A (en
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李琳琳
孙月竹
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Rushan Dayang Silica Gel Co ltd
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Rushan Dayang Silica Gel Factory
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00Silicon; Compounds thereof
    • C01B33/113Silicon oxides; Hydrates thereof
    • C01B33/12Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • C01B33/16Preparation of silica xerogels
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00Silicon; Compounds thereof
    • C01B33/113Silicon oxides; Hydrates thereof
    • C01B33/12Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • C01B33/14Colloidal silica, e.g. dispersions, gels, sols
    • C01B33/157After-treatment of gels
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/12Surface area
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/14Pore volume
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/16Pore diameter

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Dispersion Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Silicon Compounds (AREA)

Abstract

The present invention relates to a kind of production method of modified pressure-variable adsorption silica gel, which solve the technical problem that the product obtained by existing method still has much room for improvement for CO2 adsorbances, it is by sodium silicate solution and dilution heat of sulfuric acid, mixed through strengthening, neutralization reaction and generate hydrogel, the water-setting micelle steeps through a hypo acid, once wash, quadratic acid steeps, secondary washing, drag for glue, primary drying, redrying step, silica gel finished product is made, hydrogel is before a hypo acid steeps step also through performic acid, acetic acid or hydrofluoric acid treatment, in secondary washing and drag for and also pass through surfactant processing step between glue step.The present invention can be used for the preparation field of adsorption silica gel.

Description

The production method of modified pressure-variable adsorption silica gel
Technical field
The present invention relates to chemical field, specifically a kind of production method of modified pressure-variable adsorption silica gel.
Background technology
At present, A types silica gel is widely used in precision instrument, industry, medicine, food, clothes, shoes and hats and daily necessities etc. The effect for removing moisture drying, substantially reaching the moisture absorption, and to the dry absorption that removes moisture of pressure-swing absorption apparatus, due to A type silica gel The design requirement of pressure-swing absorption apparatus is not reached much to CO2 adsorption capacity, therefore can not meet to require.
Publication No. CN101053819 B are authorized the invention discloses a kind of production method of variable-pressure adsorption silica gel, its Comprise the following steps:Sodium silicate and the concentrated sulfuric acid are made into weak solution, the sodium silicate solution prepared and sulfuric acid solution carried out strong Change mixing neutralization reaction and hydrogel is made;Hydrogel aging is subjected to sour bubble, washing, by the silica gel washed for the first time hypo acid again Bubble, washing, acid content is 0.008~0.015% in silica gel after secondary washing;Jing Pao will be carried out by the silica gel washed twice After pull out, dry for the first time, dried silica gel for the first time screened, then carry out redrying, redrying is What is carried out on vibrated fluidized bed in short-term, rapidly dries, and product is made within 2% in moisture control, and the present invention has higher Specific surface area, chemical property is stable, nonpoisonous and tasteless, has the features such as stronger adsorption capacity to carbon dioxide and vapor.But Product made from this method still has much room for improvement for CO2 adsorbances.
The content of the invention
The present invention is exactly that the technology still having much room for improvement for CO2 adsorbances to solve the product obtained by existing method is asked A kind of topic, there is provided production method for the modification pressure-variable adsorption silica gel that CO2 adsorbances can be greatly improved.
Therefore, the present invention provides a kind of production method of modified pressure-variable adsorption silica gel, it is by sodium silicate solution and dilute sulfuric acid Solution, mixed through strengthening, neutralization reaction and generate hydrogel, the water-setting micelle steep through a hypo acid, once washing, quadratic acid steep, Secondary washing, glue, primary drying, redrying step are dragged for, silica gel finished product is made, hydrogel also passes through before a hypo acid steeps step Formic acid, acetic acid or hydrofluoric acid treatment.Formic acid, acetic acid or hydrofluoric acid step process are containing formic acid, acetic acid or hydrogen by water-setting micelle Soak 0.9~5 minute, entered back into hypo acid bubble liquid in the solution of fluoric acid material.The solution of formic acid, acetic acid or hydrofluoric acid material Mass percent concentration be 0.5~5.0%.
Preferably, the time of communicated band is 0.9~10 minute.
Preferably, secondary washing and described drag for also pass through surfactant processing step between glue step
Preferably, surfactant processing step is that micelle after the completion of secondary water is washed enters back into and added surface-active 5~10h of immersion treatment in agent solution.
Preferably, the mass percent concentration of surfactant solution is 0.3~0.6%.
The beneficial effects of the invention are as follows:Because the manufacture method of modified pressure-variable adsorption silica gel in the present invention is in advance in water The material of a kind of formic acid, acetic acid or hydrofluoric acid is added, is granulated to enter in the solution for latter second in silica gel and soaks, to prevent it Aging reaming, so than micropore becomes thinner in pressure-variable adsorption silica gel before modified, specific surface area is higher.The present invention is above-mentioned in entrance After being soaked in the solution, by conveyer belt aging, it is sent in hypo acid bubble liquid, so than traditional method, its micropore is not only Carefully, and uniformly, so that modified pressure-variable adsorption silica gel CO2 adsorbances reach peak;Due to the gel particles first Acid, acetic acid or hydrofluoric acid material treat, so after the drying, there is fried line on surface, in order to ensure that micelle surface nondestructive is hindered, so Surfactant processing is added, so micelle surface can not only also accordingly improved without fried line, mechanical strength.
Embodiment
According to following embodiments, the present invention may be better understood.It is however, as it will be easily appreciated by one skilled in the art that real Apply the content described by example and be merely to illustrate the present invention, without should be also without limitation on this hair described in claims It is bright.
Surfactant used is purchased from the IW dispersants of Zibo Yun Chuan Chemical Co., Ltd.s production in the present invention, and its is main Composition is AEO;In following examples, in addition to having and indicating, concentration is mass percent concentration.
Embodiment 1
The present invention generates hydrogel by sodium silicate solution and dilution heat of sulfuric acid, through strengthening mixing, neutralization reaction, the water-setting Micelle through formic acid, acetic acid or hydrofluoric acid treatment → washing → quadratic acid bubble → secondary washing → WA surfaces of a hypo acid bubble → once live Property agent handles → dragged for the PROCESS FOR TREATMENT of glue → primary drying → redrying, so as to obtain being modified pressure-variable adsorption silica gel product.
The modification pressure-variable adsorption silica gel of the present invention is on the basis of traditional pressure-variable adsorption silica gel, and preparation contains sio219% Sodium silicate solution and content be 22% sulfuric acid solution, by strengthen mix, neutralization reaction and generate water-setting micelle.Formic acid, Acetic acid or hydrofluoric acid PROCESS FOR TREATMENT be by obtained water-setting micelle in 1 second enter in advance added a kind of formic acid, acetic acid or Soaked 5 minutes in the solution of hydrofluoric acid material, then communicated band enters in hypo acid bubble liquid for 10 minutes;One hypo acid bubble processing be by Hydrogel micelle after moment burin-in process, which is immersed in 6% acid solution, handles 15h;The PROCESS FOR TREATMENT once washed is by one Glue after the completion of hypo acid bubble, in 40 DEG C of water at low temperature, it is by first to rinse into glue containing sour 0.008% quadratic acid bubble PROCESS FOR TREATMENT 15h is handled in the acid solution of micelle immersion 1% after the completion of secondary washing;Secondary washing PROCESS FOR TREATMENT is after the completion of quadratic acid is steeped Acid, washed in 40 DEG C of water at low temperature, into glue containing acid 0.01%;The processing of WA surfactants is to wash into secondary water Micelle afterwards, which enters back into, has added immersion treatment 5h in WA surfactant solutions.
Acid selected by hypo acid bubble and quadratic acid bubble technique of the invention is sulfuric acid, one kind in hydrochloric acid, nitric acid.
Embodiment 2-6
The specific technological parameters of embodiment 2-6 and test rating are as shown in table 1, and other parameters and step are the same as embodiment 1.
Comparative example
Comparative example is same as Example 6 without formic acid, acetic acid or hydrofluoric acid treatment, other steps and technological parameter.
Table 1
The modification pressure-variable adsorption silica gel of the present invention, especially suitable for chemical industry, metallurgy, petrochemical industry, machinery, electronics, food, medicine The industries such as product, light industry, environmental protection, ethene, vinyl chloride, purifying carbon oxide, carbon dioxide, carry hydrogen, carry helium, desulfurization, oxygen processed, nitrogen processed Deng field, economy, environmental protection, this product service life length, benefit protrudes.

Claims (5)

1. a kind of production method of modified pressure-variable adsorption silica gel, it mixes sodium silicate solution and dilution heat of sulfuric acid through strengthening, in With reaction and generate hydrogel, the water-setting micelle steeps through a hypo acid, once washing, quadratic acid bubble, secondary washing, drag for glue, once Dry, redrying step, silica gel finished product be made, it is characterised in that:The hydrogel also passes through first before a hypo acid steeps step Acid, acetic acid or hydrofluoric acid treatment;
The formic acid, acetic acid or hydrofluoric acid treatment are that water-setting micelle is soaked into 0.9 in the solution containing formic acid, acetic acid or hydrofluoric acid ~5 minutes, then once acid steeps in liquid the entrance of communicated band;
The mass percent concentration of the solution of the formic acid, acetic acid or hydrofluoric acid material is 0.5~5.0%.
2. the production method of modified pressure-variable adsorption silica gel according to claim 1, it is characterised in that the communicated band Time is 0.9~10 minute.
3. the production method of modified pressure-variable adsorption silica gel according to claim 1, it is characterised in that in the secondary washing And described drag for also passes through surfactant processing step between glue step.
4. the production method of modified pressure-variable adsorption silica gel according to claim 3, it is characterised in that in the surface-active Agent processing step is that the micelle after the completion of secondary water is washed enters back into and added 5~10h of immersion treatment in surfactant solution.
5. the production method of modified pressure-variable adsorption silica gel according to claim 4, it is characterised in that the surfactant Mass percent concentration be 0.3~0.6%.
CN201610662435.1A 2016-08-12 2016-08-12 The production method of modified pressure-variable adsorption silica gel Active CN106276926B (en)

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CN111334207A (en) * 2018-12-18 2020-06-26 深圳市弗雷丹尔科技有限公司 Antistatic mobile phone protection film
CN110347213B (en) * 2019-07-15 2022-12-23 深圳英芯科技有限公司 Portable computer with flexible display screen
CN110898811A (en) * 2019-12-19 2020-03-24 乳山市大洋硅胶厂 Preparation method of nitrogen adsorption silica gel
CN110918048A (en) * 2019-12-19 2020-03-27 乳山市大洋硅胶厂 Preparation method of hydrogen-absorbing pressure swing adsorption silica gel
CN113013385A (en) * 2019-12-19 2021-06-22 山西沃特海默新材料科技股份有限公司 Coating agent, silicon-carbon material and preparation process
CN110918049A (en) * 2019-12-19 2020-03-27 乳山市大洋硅胶厂 Preparation method of methane adsorption silica gel
CN111298763A (en) * 2020-03-03 2020-06-19 山东建筑大学 Modified silica gel CO2Adsorbent and preparation method and application thereof

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CN1554582A (en) * 2003-12-28 2004-12-15 王燕春 Method for producing mesoporous silicon gel
CN101224409A (en) * 2007-10-18 2008-07-23 烟台博瑞特精细化工有限公司 Production method of superfine silica powder with high adsorption value
CN102079527A (en) * 2009-11-27 2011-06-01 姜小宁 Manufacturing method of micro-powder macroporous silicon gel
CN105195087A (en) * 2015-10-26 2015-12-30 王立卓 Extra-large-aperture silicon dioxide new material and preparation method thereof

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EP1314695B1 (en) * 2001-11-27 2007-08-22 Mitsubishi Chemical Corporation Silica and method for producing the same
KR100868989B1 (en) * 2007-05-23 2008-11-17 엠파워(주) Method of fabricating superhydrophobic silica chain powders

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Publication number Priority date Publication date Assignee Title
CN1554582A (en) * 2003-12-28 2004-12-15 王燕春 Method for producing mesoporous silicon gel
CN101224409A (en) * 2007-10-18 2008-07-23 烟台博瑞特精细化工有限公司 Production method of superfine silica powder with high adsorption value
CN102079527A (en) * 2009-11-27 2011-06-01 姜小宁 Manufacturing method of micro-powder macroporous silicon gel
CN105195087A (en) * 2015-10-26 2015-12-30 王立卓 Extra-large-aperture silicon dioxide new material and preparation method thereof

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Address after: No.46, ZHUJIAZHUANG commercial road, Rushankou Town, Rushan City, Weihai City, Shandong Province

Patentee after: Rushan Dayang silica gel Co.,Ltd.

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Denomination of invention: Production method of modified pressure swing adsorption silica gel

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