CN103055860A - Composited crystal solid alkali supporter catalyst and preparation method - Google Patents
Composited crystal solid alkali supporter catalyst and preparation method Download PDFInfo
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- CN103055860A CN103055860A CN2012105878704A CN201210587870A CN103055860A CN 103055860 A CN103055860 A CN 103055860A CN 2012105878704 A CN2012105878704 A CN 2012105878704A CN 201210587870 A CN201210587870 A CN 201210587870A CN 103055860 A CN103055860 A CN 103055860A
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Abstract
The invention discloses a composited crystal solid alkali supporter catalyst and a preparation method thereof. The preparation method comprises the following steps: (1) dissolving CaCl2, AlCl3, MgCl2, Zn(NO3)2 and CdCl2 into water to obtain a solution A, dissolving NaCO3 into water to obtain a solution B, and mixing nano SrCO3 with water to obtain a solution C; (2) adding dropwise the solution A and the solution B into the solution C, stirring at the temperature of 70-80 DEG C, standing, filtrating in a suction manner, collecting precipitates, washing, drying, roasting, and grinding into powder; (3) mixing the solutions of K2CO3 and AuCl3, roasting, and grinding into powder; (4) adding the K2OSO4 solution to mix, and evaporating a solvent to obtain the composited crystal solid alkali supporter catalyst. According to the invention, the strength of the alkaline is remarkably increased, and the composited crystal solid alkali supporter catalyst is applicable to an organic synthesis reaction and can remarkably increase the yield of the chemical reaction.
Description
Technical field
The present invention relates to a kind of compound brilliant solid base carried catalyst and preparation method, should say the preparation method who generates compound brilliant solid base carried catalyst by method for crystallising.
Background technology
Solid base catalyst is the human a kind of novel catalyst of finding, high activity, high selectivity, chemical reaction condition are gentle because having, reaction system is separated easily, etching apparatus not, environmental friendliness, the advantage such as can reuse and more and more paid attention to, especially aspect synthetic at fine chemistry, the Polymer Synthesizing, make the chemosynthesis reaction of a lot of severe reaction conditions can be easy to carry out, and make the synthesis process serialization, reduced energy resource consumption, reduced the pollution to environment, in recent years the research and development of solid base also come extensively.Yet because solid base is novel catalyst, starting is evening relatively, and especially aspect the preparation solid base, preparation technology requires very meticulous, and cost is expensive, and specific area and mechanically stable intensity also are restricted because preparation technology is meticulous simultaneously.
Summary of the invention
The objective of the invention is to disclose a kind of compound brilliant solid base carried catalyst and preparation method, the defects that exists to overcome prior art.
The preparation method of compound brilliant solid base carried catalyst of the present invention comprises the steps: chemical constituent:
(1) with CaCl
2, AlCl
3, MgCl
2, Zn (NO
3)
2And CdCl
2Be dissolved in 250 parts of deionized waters, obtain A solution;
With NaCO
3Be dissolved in 250 parts of deionized waters, obtain B solution;
With nanometer SrCO
3Mix with 500 parts of deionized waters, obtain C solution;
(2) at 20 ℃～30 ℃, described A solution and described B solution are added drop-wise in the C solution simultaneously, dropwised in 20 minutes at 10 minutes, stirred 2～3 hours, and then be warming up to 70 ℃～80 ℃, continue to stir 2～3 hours, be down to normal temperature, after static 5～10 hours, suction filtration, collecting precipitation thing, washing, be dried to moisture at 100 ℃～120 ℃ and all evaporate, 1150 ℃～1250 ℃ roastings after 3～4 hours, with calcining matter grounds travel powder;
(3) with the powder of step (2), add K
2CO
3And AuCl
3After solution mixes, 950 ℃～1150 ℃ lower roastings after 1～2 hour, again with calcining matter grounds travel powder;
(4) powder with step (3) adds K again
2OsO
4After solution mixes, 90 ℃～100 ℃ lower solvent evaporated under reduced pressure of passing through, obtain compound brilliant solid base carried catalyst;
Described nanometer SrCO
3Particle diameter be 20～30 nanometers, preferred 25 nanometers;
K
2OsO
4Be the molecular formula of potassium osmate, the parts by weight of each component are:
CaCl
215～25 parts, AlCl
35～10 parts, MgCl
21～3 part, Zn (NO
3)
25～10 parts, CdCl
20.5～1.5 parts, nanometer SrCO
31～3 part, Na
2CO
320～30 parts, AuCl
3Solution 1.67%(weight) 10～20 parts, K
2CO
35～10 parts, K
2OsO
4Solution 1%(weight) 5～10 parts;
The invention reside in by crystallochemical reaction and the mode of utilizing crystal growing process to generate mixed crystal and prepare compound brilliant solid base carried catalyst, increase mixed crystal solid base specific area, utilize simultaneously the plane of crystal porous to increase the combination position that oxide surface is accepted proton, the intensity that significantly improves alkali is gone back other catalyst of load simultaneously, forms a kind of compound brilliant solid base carried catalyst.
Compound brilliant solid base carried catalyst of the present invention is by the crystallization principle in the chemical reaction process, by composite chemical reaction preparation crystal and recrystallization doping chemical reaction oxide surface is mixed and chemical coordination, impel and form mixed crystal between the oxide, enlarge specific area, increase oxide surface and accept the combination position of proton, the intensity that significantly improves alkali is other catalyst of load also, the catalyst that can be used for organic synthesis, significantly improve the yield of chemical reaction, be easy to separate, can improve product purity and product yield.
Following examples or Application Example are weight portion:
Embodiment 1
One, mixed crystal solid super base combination catalyst prepares by following steps;
(a). chemical constituent: 1000 parts of deionized waters, CaCl
215 parts, AlCl
310 parts, MgCl
21 part, Zn (NO
3)
210 parts, CdCl
20.5 part, nanometer SrCO
31 part, NaCO
330 parts, A
uCl
31.67%10 parts of solution, K
2CO
35 parts, K
2OsO
41%10 parts of solution;
(b). with CaCl
2, AlCl
3, MgCl
2And Zn (NO
3)
2And CdCl
2Be dissolved into after the mixing in 250 parts of deionized waters, with NaCO
3Be dissolved in 250 parts of deionized waters, in reactor, add 500 parts of deionized waters, add again nanometer SrCO
3, open high speed dispersor 1500 Zhuan ∕ and divide, all solution temperatures are controlled at 20 ℃, with CaCl
2, Al Cl
3, MgCl
2And Zn (NO
3)
2And CdCl
2Mixed liquor and NaCO
3The two notes of solution is added drop-wise in the reactor, dropwises in 10 minutes, and high-speed stirred is 3 hours under 20 ℃ of temperature, then be warming up to 80 ℃, continue to stir 2 hours, impel crystal size and shape to reach unanimity by intensification, stop to stir, be down to normal temperature, after static 10 hours, the suction filtration sediment cleans 3 times with 300 parts of deionized waters at every turn, foreign ion in the washing and precipitating thing, and be dried to moisture at 120 ℃ and all evaporate;
(c). with the product of (b) process, 1150 ℃ of lower roastings after 4 hours, with calcining matter grounds travel powder;
(d). with the powder of (c) process, add again K
2CO
3And A
uCl
3After solution mixes, 1150 ℃ of lower roastings after 1 hour, again with calcining matter grounds travel powder;
(e) powder with (d) process adds K again
2OsO
4After solution mixes, 90 ℃ of lower solvent evaporated under reduced pressure of passing through, obtain compound brilliant solid base carried catalyst.。
Embodiment 2
One, mixed crystal solid super base combination catalyst, its feature prepares by following steps;
(a). chemical constituent: 1000 parts of deionized waters, CaCl
225 parts, AlCl
35 parts, MgCl
23 parts, Zn (NO
3)
25 parts, CdCl
21.5 part, nanometer SrCO
33 parts, NaCO
320 parts, A
uCl
31.67%20 parts of solution, K
2CO
37.5 part, K
2OsO
41%5 parts of solution;
(b). with CaCl
2, AlCl
3, MgCl
2And Zn (NO
3)
2And CdCl
2Be dissolved into after the mixing in 250 parts of deionized waters, with NaCO
3Be dissolved in 250 parts of deionized waters, in reactor, add 500 parts of deionized waters, add again nanometer SrCO
3, open high speed dispersor 2000 Zhuan ∕ and divide, all solution temperatures are controlled at 30 ℃, with CaCl
2, AlCl
3, MgCl
2And Zn (NO
3)
2And CdCl
2Mixed liquor and NaCO
3The two notes of solution is added drop-wise in the reactor, dropwises in 20 minutes, and high-speed stirred is 2 to 3 hours under 30 ℃ of temperature, then be warming up to 70 ℃, continued high-speed stirred 3 hours, and impelled crystal size and shape to reach unanimity by intensification, stop to stir, be down to normal temperature, after static 5 hours, the suction filtration sediment cleans 3 times with 300 parts of deionized waters at every turn, foreign ion in the washing and precipitating thing, and be dried to moisture at 100 ℃ and all evaporate;
(c). with the product of (b) process, 1250 ℃ of lower roastings after 3 hours, with calcining matter grounds travel powder;
(d). with the powder of (c) process, add again K
2CO
3And A
uCl
3After solution mixes, 950 ℃ of lower roastings after 1 hour, again with calcining matter grounds travel powder;
(e) powder with (d) process adds K again
2OsO
4After solution mixes, 100 ℃ of lower solvent evaporated under reduced pressure of passing through, obtain compound brilliant solid base carried catalyst.
Embodiment 3
Mixed crystal solid super base combination catalyst, its feature prepares by following steps;
(a). chemical constituent: 1000 parts of deionized waters, CaCl
220 parts, AlCl
37.5 part, MgCl
22 parts, Zn (NO
3)
27.5 part, CdCl
21 part, nanometer SrCO
32 parts, NaCO
325 parts, A
uCl
31.67%15 parts of solution, K
2CO
310 parts, K
2OsO
41%7.5 parts of solution;
(b). with CaCl
2, AlCl
3, MgCl
2And Zn (NO
3)
2And CdCl
2Be dissolved into after the mixing in 250 parts of deionized waters, with NaCO
3Be dissolved in 250 parts of deionized waters, in reactor, add 500 parts of deionized waters, add again nanometer SrCO
3, open high speed dispersor 1750 Zhuan ∕ and divide, all solution temperatures are controlled at 25 ℃, with CaCl
2, AlCl
3, MgCl
2And Zn (NO
3)
2And CdCl
2Mixed liquor and NaCO
3The two notes of solution is added drop-wise in the reactor, dropwises in 15 minutes, and high-speed stirred is 2.5 hours under 25 ℃ of temperature, then be warming up to 75 ℃, continued high-speed stirred 2.5 hours, and impelled crystal size and shape to reach unanimity by intensification, stop to stir, be down to normal temperature, after static 7.5 hours, the suction filtration sediment cleans 3 times with 300 parts of deionized waters at every turn, foreign ion in the washing and precipitating thing, and be dried to moisture at 110 ℃ and all evaporate;
(c). with the product of (b) process, 1200 ℃ of lower roastings after 3.5 hours, with calcining matter grounds travel powder;
(d). with the powder of (c) process, add again K
2CO
3And A
uCl
3After solution mixes, 1050 ℃ of lower roastings after 1.5 hours, again with calcining matter grounds travel powder;
(e) powder with (d) process adds K again
2OsO
4After solution mixes, 95 ℃ of lower solvent evaporated under reduced pressure of passing through, obtain compound brilliant solid base carried catalyst.
Application Example
Utilize compound brilliant solid base carried catalyst composed paper ultra-violet absorber-menthyl salicylate of the present invention.
The preparation of menthyl salicylate:
Application Example 1(embodiment sample 1): in the reaction of salicylate menthyl ester, add compound brilliant solid base carried catalyst of the present invention.
Add 100 parts of gaultherolins in reactor, 100 parts of menthols add 1 part of solid base carried catalyst, are warming up to 160 ℃, 5 hours reaction time.After when being reacted to, separating solids alkali carried catalyst, then use the water-solubility impurity in the deionized water extractive reaction product, draw the upper strata transparent oily liquid, extract three times, measure the pH value of transparent oily liquid in the 7-7.5 scope, at 90 ℃ of moisture content of removing in the transparent oily liquid, after the moisture content in transparent oily liquid was removed, the cut that then is collected in 143 ℃ of-144 ℃/2.7kPa got colourless transparent liquid with distillation under vacuum, yield 78.8%, purity 98.7%
Application Example 2(embodiment sample 2): in the reaction of salicylate menthyl ester, add compound brilliant solid base carried catalyst of the present invention.
Add 100 parts of gaultherolins in reactor, 100 parts of menthols add 1 part of solid base carried catalyst, are warming up to 160 ℃, 5 hours reaction time.After when being reacted to, separating solids alkali carried catalyst, then use the water-solubility impurity in the deionized water extractive reaction product, draw the upper strata transparent oily liquid, extract three times, measure the pH value of transparent oily liquid in the 7-7.5 scope, at 90 ℃ of moisture content of removing in the transparent oily liquid, after the moisture content in transparent oily liquid was removed, the cut that then is collected in 143 ℃ of-144 ℃/2.7kPa got colourless transparent liquid with distillation under vacuum, yield 76.7%, purity 98.6%
Application Example 3(embodiment sample 3): in the reaction of salicylate menthyl ester, add compound brilliant solid base carried catalyst of the present invention.
Add 100 parts of gaultherolins in reactor, 100 parts of menthols add 1 part of solid base carried catalyst, are warming up to 160 ℃, 5 hours reaction time.After when being reacted to, separating solids alkali carried catalyst, then use the water-solubility impurity in the deionized water extractive reaction product, draw the upper strata transparent oily liquid, extract three times, measure the pH value of transparent oily liquid in the 7-7.5 scope, at 90 ℃ of moisture content of removing in the transparent oily liquid, after the moisture content in transparent oily liquid was removed, the cut that then is collected in 143 ℃ of-144 ℃/2.7kPa got colourless transparent liquid with distillation under vacuum, yield 77.2%, purity 98.7%
Comparative sample: in the reaction of salicylate menthyl ester, do not add compound brilliant solid base carried catalyst of the present invention, add Anhydrous potassium carbonate as catalyst.
Add 100 parts of gaultherolins in reactor, 100 parts of menthols add 1 part of Anhydrous potassium carbonate, are warming up to 160 ℃, 5 hours reaction time.After when being reacted to, separate potassium carbonate catalyst, then use the water-solubility impurity in the deionized water extractive reaction product, draw the upper strata transparent oily liquid, extract three times, measure the pH value of transparent oily liquid in the 7-7.5 scope, at 90 ℃ of moisture content of removing in the transparent oily liquid, after the moisture content in transparent oily liquid was removed, the cut that then is collected in 143 ℃ of-144 ℃/2.7kPa got colourless transparent liquid with distillation under vacuum, yield 70.1%, purity 98.3%.
Solid base Basicity Determination and paper see Table 1. with ultra-violet absorber-menthyl salicylate testing result
Table 1
Can find out from above-mentioned application result: use the paper of the synthetic preparation of catalyst of the present invention to compare with typical catalyst with ultra-violet absorber-menthyl salicylate, the product yield is high, catalyst effect is remarkable, the product purity advantages of higher, compound brilliant solid base carried catalyst of the present invention is described, catalytic action is remarkable, is desirable solid base carried catalyst.
Claims (6)
1. the preparation method of compound brilliant solid base carried catalyst is characterized in that, comprises the steps:
(1) with CaCl
2, AlCl
3, MgCl
2, Zn (NO
3)
2And CdCl
2Be dissolved in 250 parts of deionized waters, obtain A solution; With NaCO
3Be dissolved in 250 parts of deionized waters, obtain B solution; With nanometer SrCO
3Mix with 500 parts of deionized waters, obtain C solution;
(2) described A solution and described B solution are added drop-wise in the C solution simultaneously, stir, then be warming up to 70 ℃～80 ℃, continue to stir, be down to normal temperature, static, suction filtration, the collecting precipitation thing, washing, drying, roasting is with calcining matter grounds travel powder;
(3) with the powder of step (2), add K
2CO
3And AuCl
3Solution mixes, and roasting is again with calcining matter grounds travel powder;
(4) powder with step (3) adds K again
2OsO
4Solution mixes, and evaporating solvent obtains compound brilliant solid base carried catalyst.
2. method according to claim 1, it is characterized in that, in the step (2), at 20 ℃～30 ℃, described A solution and described B solution are added drop-wise in the C solution simultaneously, dropwised in 20 minutes at 10 minutes, stirred 2～3 hours, then be warming up to 70 ℃～80 ℃, continue to stir 2～3 hours, be down to normal temperature, after static 5～10 hours, suction filtration, the collecting precipitation thing, washing is dried to moisture at 100 ℃～120 ℃ and all evaporates, 1150 ℃～1250 ℃ roastings after 3～4 hours, with calcining matter grounds travel powder.
3. method according to claim 1 is characterized in that, in the step (3), with the powder of step (2), adds K
2CO
3And AuCl
3After solution mixes, 950 ℃～1150 ℃ lower roastings after 1～2 hour, again with calcining matter grounds travel powder.
4. method according to claim 1 is characterized in that, described nanometer SrCO
3Particle diameter be 20～30 nanometers.
5. each described method is characterized in that according to claim 1～4, and the parts by weight of each component are: CaCl
215～25 parts, AlCl
35～10 parts, MgCl
21～3 part, Zn (NO
3)
25～10 parts, CdCl
20.5～1.5 parts, nanometer SrCO
31～3 part, Na
2CO320～30 part, AuCl
3Solution 1.67%(weight) 10～20 parts, K
2CO
35～10 parts, K
2OsO
4Solution 1%(weight) 5～10 parts.
6. the compound brilliant solid base carried catalyst of each described method preparation according to claim 1～5.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103406134A (en) * | 2013-07-09 | 2013-11-27 | 上海东升新材料有限公司 | Aluminum oxide carrier solid alkali catalyst and preparation method thereof |
| CN104014338A (en) * | 2014-06-12 | 2014-09-03 | 上海东升新材料有限公司 | Solid alkali carrier rare metal element catalyst and preparation method thereof |
| CN111876597A (en) * | 2020-08-03 | 2020-11-03 | 国家地质实验测试中心 | Extraction of radioactive cause from molybdenite187Methods for Os |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030152510A1 (en) * | 2001-11-15 | 2003-08-14 | Ernest Senderov | TS-PQ titano-silicate molecular sieves and methods for synthesis and use thereof |
| CN102247827A (en) * | 2011-05-04 | 2011-11-23 | 湖南大学 | Novel nano solid super-strong alkali catalyst and preparation and application thereof |
-
2012
- 2012-12-28 CN CN201210587870.4A patent/CN103055860B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030152510A1 (en) * | 2001-11-15 | 2003-08-14 | Ernest Senderov | TS-PQ titano-silicate molecular sieves and methods for synthesis and use thereof |
| CN102247827A (en) * | 2011-05-04 | 2011-11-23 | 湖南大学 | Novel nano solid super-strong alkali catalyst and preparation and application thereof |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103406134A (en) * | 2013-07-09 | 2013-11-27 | 上海东升新材料有限公司 | Aluminum oxide carrier solid alkali catalyst and preparation method thereof |
| CN103406134B (en) * | 2013-07-09 | 2016-02-10 | 上海东升新材料有限公司 | Preparation method of a kind of Aluminum oxide carrier solid alkali catalyst and products thereof |
| CN104014338A (en) * | 2014-06-12 | 2014-09-03 | 上海东升新材料有限公司 | Solid alkali carrier rare metal element catalyst and preparation method thereof |
| CN104014338B (en) * | 2014-06-12 | 2016-03-02 | 上海东升新材料有限公司 | Solid base carrier thallium catalyst and preparation method |
| CN111876597A (en) * | 2020-08-03 | 2020-11-03 | 国家地质实验测试中心 | Extraction of radioactive cause from molybdenite187Methods for Os |
| CN111876597B (en) * | 2020-08-03 | 2022-02-22 | 国家地质实验测试中心 | Extraction of radioactive cause from molybdenite187Methods for Os |
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