CN104261444A - Zero-discharge method for one-step direct synthesis of magnesium-aluminum hydrotalcite - Google Patents

Zero-discharge method for one-step direct synthesis of magnesium-aluminum hydrotalcite Download PDF

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Publication number
CN104261444A
CN104261444A CN201410492050.6A CN201410492050A CN104261444A CN 104261444 A CN104261444 A CN 104261444A CN 201410492050 A CN201410492050 A CN 201410492050A CN 104261444 A CN104261444 A CN 104261444A
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magnesium
hydrotalcite
aluminum hydrotalcite
suspension
alumina
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苏继新
孙明明
肖煜昕
高雪
张�林
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Shandong University
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Shandong University
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F7/00—Compounds of aluminium
    • C01F7/78—Compounds containing aluminium and two or more other elements, with the exception of oxygen and hydrogen

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Inorganic Chemistry (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)

Abstract

The invention discloses a zero-discharge method for one-step direct synthesis of magnesium-aluminum hydrotalcite. The method comprises the following steps: (1) weighing alumina sol and light magnesium oxide according to the magnesium-aluminum molar ratio of (1:1) to (5:1), mixing and then adding deionized water to prepare suspension liquid, so that the weight ratio of the solid content in the suspension liquid is 15.3%-34.7%; (2) enabling the suspension liquid to react and peptize at the temperature of 20-100 DEG for 3-48 hours, so as to prepare magnesium-aluminum hydrotalcite sol; and (3) drying the obtained magnesium-aluminum hydrotalcite sol, so as to obtain the product in a dry state. According to the method, no excessive soluble salt is added, the magnesium-aluminum hydrotalcite is directly prepared by adopting a one-step mixing reaction method, no wastewater and waste salt are discharged, the raw materials are all transformed into the product, and the method is a low-cost, green and clean synthesis process which accords with the characteristics of atom economy.

Description

A kind of zero release one step directly synthesizes the method for magnesia-alumina hydrotalcite
Technical field
The present invention relates to a kind of method for the synthesis of magnesia-alumina hydrotalcite, belong to magnesia-alumina hydrotalcite synthesis technical field.
Background technology
The anionic clay of hydrotalcite one quasi-representative, its synthetic method and applied research receive to be paid attention to widely, has had numerous research reports and patent application.Compared with applying with the broad scale research of cationic clay; the application of houghite still receives the restriction of each side factor; one of major reason is wherein that natural houghite ore deposit is less, and the product that commercial synthesis obtains is by raw material, environment protection reason, the restriction that cost is higher.
The synthetic method of hydrotalcite is more, wherein co-precipitation, washing, hydrothermal treatment consists are the methods commonly used the most, the method technique is simple, product crystal formation is good, but under the situation of environmental regulation increasingly stringent, production process can produce a large amount of waste water, and has a large amount of salts in waste water, cause cost for wastewater treatment high, abraum salt such as cannot to process at numerous difficult problem.For decreasing pollution, reduce costs, existing a lot of achievement in research is devoted to solve the problem, " for the SO reduced from FCC revivifier disclosed in Chinese patent literature CN101687660A xthe anionic clay containing additive of discharge and preparation technology thereof ", propose the physical mixture of grinding bivalent metallic compound and trivalent metal compound, at the physical mixture that the temperature lower calcinations of 200 DEG C to about 800 DEG C are ground, and make burnt mixture rehydrated with the anionic clay method formed containing additive in aq suspension, avoid above-mentioned waste water, the having problems of abraum salt, but required equipment is complicated, high-temperature calcination cost is higher.
CN1507944A disclosed " a kind of clean synthesis method of magnesium aluminum-hydrotalcite ", with MgCO 3or M g(OH) 2for magnesium source, 400-900 DEG C of roasting 3-5 hour, produces active MgO, then mixes with sodium aluminate aqueous solution, and Mg/Al molar ratio is 1.0-4.5, adds NaOH and Na 2cO 3, its mol ratio NaOH/NaOH+Na 2cO 3for 0.7-0.9, pH value controls at 10-12,60-100 DEG C of stirring lower reaction 4-15 hour, and product filtration, washing, drying, namely obtain the magnesium aluminum-hydrotalcite that thing is mutually single.Wherein the process such as filtration, washing of product still cannot avoid a large amount of generations of waste water completely.
CN101229927A disclosed " a kind of water-heat one-step synthesis of nanocrystalline Mg-Al hydrotalcite ", with MgO, Al (OH) 3, and Na 2cO 3for synthesis initiator, in autogenous pressure still, the nanocrystalline single-phase Mg-Al hydrotalcite of one-step synthesis is a kind of significant exploration, but the problem of the method still unresolved waste water, abraum salt, and the high expensive of high-temperature water thermal means.
In addition CN102139902B disclosed " method of synthesizing magnesia-alumina spinel by roasting chloride ion type Mg-Al hydrotalcite at low temperature " and CN102863043B disclosed " organic hydrotalcite synthesis and wastewater treatment integral process " etc. is also had.Capital produces waste water, abraum salt discharge.
Summary of the invention
The present invention is directed to the deficiency that existing magnesia-alumina hydrotalcite synthetic technology exists, propose a kind of without waste water, abraum salt discharge, raw material is all converted into product, accords with low cost, and green clean zero release one step directly synthesizes the method for magnesia-alumina hydrotalcite.
Zero release one step of the present invention directly synthesizes the method for magnesia-alumina hydrotalcite, comprises the following steps:
(1) take Alumina gel and light magnesium oxide according to the ratio of magnalium mol ratio 1:1-5:1, add deionized water after mixing and make suspension, make the weight ratio of the solid content in suspension be 15.3%-34.7%;
(2) by suspension at 20-100 DEG C of temperature, reaction peptization 3 hours-48 hours, obtained magnesia-alumina hydrotalcite colloidal sol;
(3) gained magnesia-alumina hydrotalcite colloidal sol is dry, namely obtain the product of drying regime.
Alumina gel is the Alumina gel of chloride, nitrate radical or sulfate radical.
The present invention does not add unnecessary soluble salt, takes a step hybrid reaction method directly to produce magnesia-alumina hydrotalcite, and have without waste water, abraum salt discharge, raw material is all converted into product, meets the low cost of the feature of atom economy, green clean synthesis process.
Embodiment
Embodiment 1: synthesis magnalium is than the houghite MgAl (OH) of 1:1 4.41cl 0.59.xH 2o
Get 200ml Alumina gel, this Alumina gel is containing aluminium 11.5% (mass ratio), Al/Cl (mass ratio)=1.3, proportion d=1.35, pH=4, add 46g light magnesium oxide, after mixing, add 400ml deionized water (in suspension, the weight ratio of solid content is 21.94% (147/ (400+200*1.35)=21.94%)) again, 70 DEG C of constant temperature 5 hours, 105 DEG C of dryings, can obtain more than the houghite MgAl (OH) of 147g magnalium than 1:1 4.41cl 0.59.xH 2o.
Embodiment 2: synthesis magnalium is than the houghite Mg of 2:1 2al (OH) 6.41cl 0.59.xH 2o
Get 200ml Alumina gel, this Alumina gel is containing aluminium 11.5% (mass ratio), Al/Cl (mass ratio)=1.3, proportion d=1.35, pH=4, add 92g light magnesium oxide, after mixing, then add 320ml deionized water (in suspension, the weight ratio of solid content is 34.7%), 100 DEG C of constant temperature 3 hours, 105 DEG C of dryings, can obtain more than the houghite Mg of 204.9g magnalium than 2:1 2al (OH) 6.41cl 0.59.xH 2o.
Embodiment 3: synthesis magnalium is than the houghite Mg of 3:1 3al (OH) 8.41cl 0.59.xH 2o
Get 200ml Alumina gel, this Alumina gel is containing aluminium 11.5% (mass ratio), Al/Cl (mass ratio)=1.3, proportion d=1.35, pH=4, add 138g light magnesium oxide, after mixing, then add 1450ml deionized water (in suspension, the weight ratio of solid content is 15.3%), 20 DEG C of constant temperature 48 hours, 105 DEG C of dryings, can obtain more than the houghite Mg of 262.9g magnalium than 3:1 3al (OH) 8.41cl 0.59.xH 2o.
Embodiment 4: synthesis magnalium is than the houghite Mg of 5:1 5al (OH) 12.41cl 0.59.xH 2o
Get 200ml Alumina gel, this Alumina gel is containing aluminium 11.5% (mass ratio), Al/Cl (mass ratio)=1.3, proportion d=1.35, pH=4, add 230g light magnesium oxide, after mixing, then add 1100ml deionized water (in suspension, the weight ratio of solid content is 27.4%), 40 DEG C of constant temperature 18 hours, 105 DEG C of dryings, can obtain more than the houghite Mg of 375.9g magnalium than 5:1 3al (OH) 8.41cl 0.59.xH 2o.
Embodiment 5
Get 200ml Alumina gel, this Alumina gel contains aluminium 11% (mass ratio), Al/NO - 3(mass ratio)=0.6, proportion d=1.45, pH=3.7, add 70.89g light magnesium oxide, after mixing, then add 400ml deionized water (in suspension, the weight ratio of solid content is 28.7%), 60 DEG C of constant temperature 7 hours, 105 DEG C of dryings, can obtain more than the houghite Mg of 198.1g magnalium than 1.5:1 1.5al (OH) 5.31(N0 3) 0.69.xH 2o.
Embodiment 6
Get 200ml Alumina gel, this Alumina gel contains aluminium 11% (mass ratio), Al/NO - 3(mass ratio)=0.6, proportion d=1.45, pH=3.7, add 118.1g light magnesium oxide, after mixing, then add 500ml deionized water (in suspension, the weight ratio of solid content is 32.4%), 80 DEG C of constant temperature 4 hours, 105 DEG C of dryings, can obtain more than the houghite Mg of 256.2g magnalium than 2.5:1 2.5al (OH) 7.31(N0 3) 0.69.xH 2o.
Embodiment 7
Get 200ml Alumina gel, this Alumina gel contains aluminium 11.2% (mass ratio), Al/SO 2- 4(mass ratio)=0.61, proportion d=1.40, pH=3.4, add 185.8g light magnesium oxide, after mixing, then add 1000ml deionized water (in suspension, the weight ratio of solid content is 26.4%), 30 DEG C of constant temperature 45 hours, 105 DEG C of dryings, can obtain more than the houghite Mg of 338.5g magnalium than 4:1 4al (OH) 10.08(S0 4) 0.46.xH 2o.

Claims (1)

1. zero release one step directly synthesizes a method for magnesia-alumina hydrotalcite, it is characterized in that, comprises the following steps:
(1) take Alumina gel and light magnesium oxide according to the ratio of magnalium mol ratio 1:1-5:1, add deionized water after mixing and make suspension, make the weight ratio of the solid content in suspension be 15.3%-34.7%;
(2) by suspension at 20-100 DEG C of temperature, reaction peptization 3 hours-48 hours, obtained magnesia-alumina hydrotalcite colloidal sol;
(3) gained magnesia-alumina hydrotalcite colloidal sol is dry, namely obtain the product of drying regime.
CN201410492050.6A 2014-09-23 2014-09-23 Zero-discharge method for one-step direct synthesis of magnesium-aluminum hydrotalcite Pending CN104261444A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1337920A (en) * 1999-01-29 2002-02-27 阿克佐诺贝尔公司 Process for producing anionic clay using boehmite
CN1370133A (en) * 1999-08-11 2002-09-18 阿克佐诺贝尔公司 Polytype Mg-Al hydrotalcite
CN102371150A (en) * 2010-08-26 2012-03-14 中国石油化工股份有限公司 Composition for reducing discharge of NOx in regeneration flue gas of fluid catalytic cracking (FCC)

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1337920A (en) * 1999-01-29 2002-02-27 阿克佐诺贝尔公司 Process for producing anionic clay using boehmite
CN1370133A (en) * 1999-08-11 2002-09-18 阿克佐诺贝尔公司 Polytype Mg-Al hydrotalcite
CN102371150A (en) * 2010-08-26 2012-03-14 中国石油化工股份有限公司 Composition for reducing discharge of NOx in regeneration flue gas of fluid catalytic cracking (FCC)

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
段明杰: "水滑石的制备及其对N2O分解的催化性能研究", 《中国优秀硕士学位论文全文数据库 工程科技I辑》, no. 01, 15 January 2014 (2014-01-15) *

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Application publication date: 20150107