CN102631940A - Composite catalyst and application thereof in preparing pale rosin glyceride - Google Patents

Composite catalyst and application thereof in preparing pale rosin glyceride Download PDF

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CN102631940A
CN102631940A CN2012100887139A CN201210088713A CN102631940A CN 102631940 A CN102631940 A CN 102631940A CN 2012100887139 A CN2012100887139 A CN 2012100887139A CN 201210088713 A CN201210088713 A CN 201210088713A CN 102631940 A CN102631940 A CN 102631940A
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composite catalyst
rosin
preparation
roasting
composite
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CN102631940B (en
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曾玉凤
蒙春玲
秦祖赠
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Yulin Normal University
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Yulin Normal University
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Abstract

The invention discloses a composite catalyst and application thereof in preparing pale rosin glyceride. The composite catalyst is prepared by the following steps: by using tetraethyl orthosilicate as a silicon source, cetyl trimethyl ammonium bromide as a template and aluminum oxide as an aluminum source, regulating the pH value with ammonia water, crystallizing, filtering, washing and roasting to obtain binary composite oxides SiO2/Al2O3; soaking the binary composite oxides in a phosphorous acid solution, filtering, drying, roasting and the like to obtain a composite catalyst-ternary composite oxides P2O5/SiO2/Al2O3; and reacting at high temperature to prepare the pale rosin glyceride by using the composite catalyst as the catalyst under the protection of nitrogen. Compared with the past preparation technique, the invention greatly shortens the esterifying reaction time, lowers the chroma of the esterified product and enhances the softening point.

Description

A kind of composite catalyst and the application in preparation pale rosin glyceride thereof
Technical field
The invention belongs to the rosin processing technique field, be specifically related to a kind of composite catalyst and the application in preparation pale rosin glyceride thereof.
Background technology
Rosin is a kind of natural reproducible resin, is made up of various isomeric resin acids, and its general molecular formula is C 19H 19COOH mostly has one the three luxuriant and rich with fragrance skeleton of ring, contains two two keys and a carboxyl.Because the double bond structure in the rosin acid; Make its easy oxidation stain, and the monobasic carboxyl in the rosin acid makes its acid number high; Easily with paint in heavy metallic salt and the metal surface that is coated with by lacquer react; Limit it and in industry, use,, need carry out modification to rosin and handle in order to overcome above-mentioned shortcoming.Esterification modification is one of means most important and the most basic in the numerous method of modifying of rosin.Behind rosin esterification, not only reduce acid number, improved heat endurance, and strengthened acidproof, the alkaline-resisting ability of rosin, be widely used in the industry such as adhesive, printing ink, coating, food and scaling powder.
Because the carbonyl of resin acid is connected on the tertiary carbon; Sterically hindered big, reaction activity is high, and esterification needs in higher reaction temperature; Could accomplish for a long time; And pyroreaction makes its easy decarboxylation for a long time, and two key oxidation stains are so esterification needs under catalyst action, to carry out usually.
Catalyst for esterification reaction mainly will have following several types: 1. bronsted acid catalyst, though lowered esterification time, colourity still Ghana's look 7 or more than, and easy decarboxylation, the softening point of product is on the low side, corrosion reaction equipment etc. limit its use; 2. solid acid catalyst, like zinc oxide, nano zine oxide, solid super-strong acid, alkyl tin acid, cerous sulfate, rare-earth oxide etc., wherein the zinc oxide effect is better, but the colourity of esterification products is appointed and is not so reached requirement; 3. organic composite catalyst, like phosphate, phenols sulfide and their mixture etc., it effectively raises reaction rate, and reaction time of esterification is shortened in a large number, and therefore the people that color reaches basically are used widely to the requirement of pale rosin fat.But, owing to added elements such as sulphur, phosphorus, influence its follow-up use, and the sulphur of pyrolytic, niff produced.
The method of producing pale rosin glyceride mainly contains two types.One of method at first prepares pale rosin, like disproportionated rosin; Foral; Perhaps utilize physics (like distillation, adsorption bleaching etc.) and chemical method (concentrated sulfuric acid decoloring method, interpolation decolorizer etc.) refined light-color rosin, direct esterification or esterification under the catalytic action of inorganic matter then, the problem of existence is that reaction temperature is high; Esterification time is long, and product colour is dark partially; Method two is rosin and glycerine direct esterification under the effect of the compound organic matter (being mainly phosphate, phenols sulfide compound) that decolorizer, antioxidant, catalyst are formed; The method cost is higher, and the ester gum color of production is than increasing under the situation that does not add catalyst.
One Chinese patent application number: CN200810026951.0; Patent name: disclose composite catalyst in the patent application document of a kind of composite catalyst and the application in the preparation light-colored rosin esters thereof, comprised the component of following mass parts: 1~200 part of hypophosphorous acid and/or hypophosphites, 1~100 part of sulfur-bearing slaine, 2~100 parts of organic disproportionation catalysts, 2~100 parts of esterification catalysts.Though this invention has been prepared solid Ghana look and has been not more than 2 light-colored rosin esters, has met light standard, has added element sulphur, at high temperature sulphur content is separated and can be produced niff, can influence its follow-up use.
Therefore study a kind of low production cost, when being used to produce pale rosin glyceride, the catalyst that product can be up to state standards again is an important research project, because active good catalyst is one of important method of shortening reaction time, raising color grade.
Summary of the invention
The objective of the invention is that to prepare in the process colourity higher in order to overcome the ester gum that exists in the prior art, residual organic catalyst, shortcomings such as production cost height; And a kind of composite catalyst is provided, it is easily separated, stable in properties; Be used for preparing the ester gum process; Technology is simple, can shorten the production time, and with low cost.
Technical scheme of the present invention:
A kind of composite catalyst, the raw material components and the weight proportion that are used to prepare the composite catalyst of pale rosin glyceride are: positive tetraethyl orthosilicate: softex kw: aluminium oxide=1: 0.3 ~ 0.6: 0.1 ~ 0.3.
The preparation method of composite catalyst of the present invention is:
(1) mixed raw material is equipped with colloidal sol: taking by weighing raw material by proportioning, is that silicon is former with positive tetraethyl orthosilicate, is template with the softex kw, and aluminium oxide is that aluminium is former, adds ammoniacal liquor then and mixes adjusting PH to 8 ~ 9; Stir and form colloidal sol;
(2) binary composite oxides preparation: colloidal sol moves in the teflon-lined stainless steel reactor, and sealing then through crystallization, is filtered, washing, and roasting makes the binary composite oxides, and main component is SiO 2And Al 2O 3
(3) ternary compound oxides preparation: the binary composite oxides are through 0.5 ~ 1molL -1Phosphorous acid solution is soaked 24 ~ 36 h, and suction filtration is removed unnecessary phosphorous acid solution, and dry 10 ~ 12 hours, behind 450 ~ 550 ℃ of following roasting 2 ~ 4 h, obtain the composite catalyst of ternary compound oxides then, main component is P 2O 5/ SiO 2/ Al 2O 3
Said crystallization is meant and colloidal sol is placed 100 ~ 130 ℃ baking oven crystallization 48 ~ 60 h; Crystalline solid product and the mother liquor isolated by filtration of said filtration after with crystallization; Said washing is that the crystalline solid product is spent deionised water to neutral, prevents its secondary crystallization; Said roasting is meant that the crystalline solid product after the washing obtains the binary composite oxides behind roasting 2 ~ 4 h in the Muffle furnace of rearmounted 450 ~ 600 ℃ of 55 ~ 65 ℃ of down dry 11 ~ 13 h.
The application of composite catalyst of the present invention in preparation pale rosin glyceride, the processing step of preparation pale rosin glyceride is: earlier rosin and said composite catalyst are placed in the reaction vessel, closed reactor vacuumized 20 ~ 30 minutes; Feed nitrogen then as protective gas, be heated to rosin all after the fusion, stir; Rotating speed is 120r/s, when temperature is increased to 170 ~ 190 ℃, adds glycerine; Be warmed up to 260 ~ 280 ℃ then, insulation reaction 3 ~ 5 hours starts vavuum pump and extracts low-boiling-point substance out; Low-boiling-point substance is cooled to 210 ~ 230 ℃ of dischargings after extracting out and accomplishing, and filters while hot, obtains pale rosin glyceride.
The weight ratio of said rosin and composite catalyst is 1: 0.001 ~ 0.005, and the weight ratio of rosin and glycerine is 1: 0.1 ~ 0.12.
Ternary compound oxides P 2O 5/ SiO 2/ Al 2O 3Be solid acid catalyst, solid acid has been widely used in the reactions such as organic chemical reactions such as esterification, disproportionation, polymerization owing to its highly acid.P 2O 5/ SiO 2/ Al 2O 3The esterification that is used for rosin and glycerine, one of its effect is a catalytic esterification, improves the efficient of esterification, has shortened the time of esterification, has reduced the oxidized probability of rosin; Two of its effect is P 2O 5/ SiO 2/ Al 2O 3The disproportionation catalytic action makes the intramolecular hydrogen atom of rosin take place to shift or remove, and produces reducing atmosphere, makes coloring matter be reduced to colourless substance.Simultaneously, esterification is carried out under the protection of nitrogen gas in anaerobic, and rosin has from discoloration under the protection of nitrogen gas, under the synergy of the two, so the ester gum lighter color of producing originally in anaerobic.
Advantage of the present invention:
1, composite catalyst preparation technology of the present invention is simple, and raw material sources are extensive.
2, adopt composite catalyst of the present invention to prepare in the pale rosin glyceride process, the consumption of composite catalyst is considerably less, and production cost effectively reduces, and catalyst is easy to separate.
3, composite catalyst of the present invention is used for preparing pale rosin glyceride process, and production technology is simple, can shorten esterification time greatly; Advantages such as it is low that the ester gum of producing has colourity, and softening point is high, and acid number is low; With low cost, have good application prospects.
4, composite catalyst of the present invention consumption in preparation pale rosin glyceride is little, and light effect is remarkable.
Specific embodiment
The present invention describes with the following example, but does not limit the scope of the invention.
Embodiment 1
1, composite catalyst P 2O 5/ SiO 2/ Al 2O 3Preparation
1. used raw material weight proportioning: positive tetraethyl orthosilicate: softex kw: aluminium oxide is 1:0.5: 0.1,
2. positive tetraethyl orthosilicate, softex kw, aluminium oxide are joined in the beaker in proportion, using ammoniacal liquor to transfer pH is 8, and normal temperature stirs down and formed colloidal sol in 2 hours; Colloidal sol is moved in the teflon-lined stainless steel reactor; The sealing, in baking oven in 120 ℃, crystallization 48 h; Crystallization is separated the crystalline solid product after finishing with mother liquor, spend deionised water to neutral; At 60 ℃ of drying 12 h, product is 500 ℃ of roasting 3 h in Muffle furnace, binary composite oxides SiO again 2/ Al 2O 3Use 0.5molL -1Phosphorous acid solution is soaked SiO 2/ Al 2O 324h, suction filtration, 60 ℃ of dry 12h, 450 ℃ of roasting 3h obtain ternary compound oxides P 2O 5/ SiO 2/ Al 2O 3, be composite catalyst of the present invention.
2, the preparation of pale rosin glyceride
Composite catalyst P with the above-mentioned preparation of 0.16g 2O 5/ SiO 2/ Al 2O 3Join in the four-hole boiling flask of the 250ml of having thermometer, mechanical agitator, nitrogen breather pipe and condenser pipe with 80g rosin, airtight, vacuumize; Feed nitrogen, vacuumize again, feed nitrogen then as protection gas; Heating rosin starts electric mixer, when temperature is elevated to 180 ℃ after all having fused; Add 9.5ml glycerine, be warmed up to 270 ℃ of insulation reaction 3 hours then, stop to feed nitrogen; The open vacuum pump is with extracting low-boiling point material half an hour out, and logical at last nitrogen is cooled to 220 ℃ of dischargings.The product softening point is 100.5 ℃, and Ghana's look 3, acid number are 14.77 (mgKOH/g)
The softening point measurement method adopts ring and ball method, and look level assay method adopts Ghana's colorimetric method for determining by standard GB/T1772-92 regulation.Acid number national standard (GB 1028-88) prescriptive procedure is measured.
Embodiment 2
1, composite catalyst P 2O 5/ SiO 2/ Al 2O 3Preparation
1. used raw material weight proportioning: positive tetraethyl orthosilicate: softex kw: aluminium oxide is 1:0.5: 0.1,
2. positive tetraethyl orthosilicate, softex kw, aluminium oxide are joined in the beaker in proportion, using ammoniacal liquor to transfer pH is 9, and normal temperature stirs down and formed colloidal sol in 2 hours; Colloidal sol is moved in the teflon-lined stainless steel reactor; The sealing, in baking oven in 110 ℃, crystallization 50 h; Crystallization is separated the crystalline solid product after finishing with mother liquor, spend deionised water to neutral; At 55 ℃ of drying 13 h, product is 550 ℃ of roasting 3 h in Muffle furnace, binary composite oxides SiO again 2/ Al 2O 3Use 0.5molL -1Phosphorous acid solution is soaked SiO 2/ Al 2O 328h, suction filtration, 65 ℃ of dry 11h, 450 ℃ of roasting 3.5h obtain ternary compound oxides P 2O 5/ SiO 2/ Al 2O 3, be composite catalyst of the present invention.
2, the preparation of pale rosin glyceride
Composite catalyst P with the above-mentioned preparation of 0.16g 2O 5/ SiO 2/ Al 2O 3Join in the four-hole boiling flask of the 250ml of having thermometer, mechanical agitator, nitrogen breather pipe and condenser pipe with 80g rosin, airtight, vacuumize; Feed nitrogen, vacuumize again, feed nitrogen then as protection gas; Heating rosin starts electric mixer, when temperature is elevated to 170 ℃ after all having fused; Add 9.5ml glycerine, be warmed up to 260 ℃ of insulation reaction 5 hours then, stop to feed nitrogen; The open vacuum pump is with extracting low-boiling point material half an hour out, and logical at last nitrogen is cooled to 210 ℃ of dischargings.
The softening point of product is 101 ℃, and Ghana's look 3, acid number are 8.86 (mgKOH/g).
The softening point measurement method adopts ring and ball method, and look level assay method adopts Ghana's colorimetric method for determining by standard GB/T1772-92 regulation.Acid number national standard (GB 1028-88) prescriptive procedure is measured.
Embodiment 3
1, composite catalyst P 2O 5/ SiO 2/ Al 2O 3Preparation
1. used raw material weight proportioning: positive tetraethyl orthosilicate: softex kw: aluminium oxide is 1:0.5:0.2,
2. positive tetraethyl orthosilicate, softex kw, aluminium oxide are joined in the beaker in proportion, using ammoniacal liquor to transfer pH is 8.5, and normal temperature stirs down and formed colloidal sol in 2 hours; Colloidal sol is moved in the teflon-lined stainless steel reactor; The sealing, in baking oven in 130 ℃, crystallization 60 h; Crystallization is separated the crystalline solid product after finishing with mother liquor, spend deionised water to neutral; At 65 ℃ of dry 11h, product is 600 ℃ of roasting 2.5 h in Muffle furnace, binary composite oxides SiO again 2/ Al 2O 3Use 0.5molL -1Phosphorous acid solution is soaked SiO 2/ Al 2O 326h, suction filtration, 65 ℃ of dry 11h, 500 ℃ of roasting 2.5h obtain ternary compound oxides P 2O 5/ SiO 2/ Al 2O 3, be composite catalyst of the present invention.
2, the preparation of pale rosin glyceride
Composite catalyst P with the above-mentioned preparation of 0.16g 2O 5/ SiO 2/ Al 2O 3Join in the four-hole boiling flask of the 250ml of having thermometer, mechanical agitator, nitrogen breather pipe and condenser pipe with 80g rosin, airtight, vacuumize; Feed nitrogen, vacuumize again, feed nitrogen then as protection gas; Heating rosin starts electric mixer, when temperature is elevated to 190 ℃ after all having fused; Add 9.5ml glycerine, be warmed up to 280 ℃ of insulation reaction 4 hours then, stop to feed nitrogen; The open vacuum pump was extracted low-boiling point material out with 20 minutes, and logical at last nitrogen is cooled to 230 ℃ of dischargings.
The softening point of product is 101 ℃, and Ghana's look 3, acid number are 7.09 (mgKOH/g).
The softening point measurement method adopts ring and ball method, and look level assay method adopts Ghana's colorimetric method for determining by standard GB/T1772-92 regulation.Acid number national standard (GB 1028-88) prescriptive procedure is measured.
Embodiment 4
1, composite catalyst P 2O 5/ SiO 2/ Al 2O 3Preparation
1. used raw material weight proportioning: positive tetraethyl orthosilicate: softex kw: aluminium oxide is 1:0.5:0.1,
2. positive tetraethyl orthosilicate, softex kw, aluminium oxide are joined in the beaker in proportion, using ammoniacal liquor to transfer pH is 8, and normal temperature stirs down and formed colloidal sol in 2 hours; Colloidal sol is moved in the teflon-lined stainless steel reactor; The sealing, in baking oven in 115 ℃, crystallization 48 h; Crystallization is separated the crystalline solid product after finishing with mother liquor, spend deionised water to neutral; At 60 ℃ of drying 12 h, product is 550 ℃ of roasting 3 h in Muffle furnace, binary composite oxides SiO again 2/ Al 2O 3Use 0.5molL -1Phosphorous acid solution is soaked SiO 2/ Al 2O 324h, suction filtration, 65 ℃ of dry 11h, 450 ℃ of roasting 3h obtain ternary compound oxides P 2O 5/ SiO 2/ Al 2O 3, be composite catalyst of the present invention.
2, the preparation of ester gum
Composite catalyst P with the above-mentioned preparation of 0.24g 2O 5/ SiO 2/ Al 2O 3Join in the four-hole boiling flask of the 250ml of having thermometer, mechanical agitator, nitrogen breather pipe and condenser pipe with 80g rosin, airtight, vacuumize; Feed nitrogen, vacuumize again, feed nitrogen then as protection gas; Heating rosin starts electric mixer, when temperature is elevated to 180 ℃ after all having fused; Add 9.5ml glycerine, be warmed up to 270 ℃ of insulation reaction 5 hours then, stop to feed nitrogen; The open vacuum pump is with extracting low-boiling point material half an hour out, and logical at last nitrogen is cooled to 220 ℃ of dischargings.
The softening point of product is 101 ℃, and Ghana's look 3, acid number are 9.26 (mgKOH/g).
The softening point measurement method adopts ring and ball method, and look level assay method adopts Ghana's colorimetric method for determining by standard GB/T1772-92 regulation.Acid number national standard (GB 1028-88) prescriptive procedure is measured.
Embodiment 5
1, composite catalyst P 2O 5/ SiO 2/ Al 2O 3Preparation
1. used raw material weight proportioning: positive tetraethyl orthosilicate: softex kw: aluminium oxide is 1:0.5:0.3,
2. positive tetraethyl orthosilicate, softex kw, aluminium oxide are joined in the beaker in proportion, using ammoniacal liquor to transfer pH is 8.5, and normal temperature stirs down and formed colloidal sol in 2 hours; Colloidal sol is moved in the teflon-lined stainless steel reactor; The sealing, in baking oven in 120 ℃, crystallization 48 h; Crystallization is separated the crystalline solid product after finishing with mother liquor, spend deionised water to neutral; At 60 ℃ of drying 12 h, product is 550 ℃ of roasting 3 h in Muffle furnace, binary composite oxides SiO again 2/ Al 2O 3Use 1molL -1Phosphorous acid solution is soaked SiO 2/ Al 2O 336h, suction filtration, 60 ℃ of dry 12h, 450 ℃ of roasting 3h obtain ternary compound oxides P 2O 5/ SiO 2/ Al 2O 3, be composite catalyst of the present invention.
2. the preparation of ester gum
Composite catalyst P with the above-mentioned preparation of 0.16g 2O 5/ SiO 2/ Al 2O 3Join in the four-hole boiling flask of the 250ml of having thermometer, mechanical agitator, nitrogen breather pipe and condenser pipe with 80g rosin, airtight, vacuumize; Feed nitrogen, vacuumize again, feed nitrogen then as protection gas; Heating rosin starts electric mixer, when temperature is elevated to 180 ℃ after all having fused; Add 8.0 ml glycerine, be warmed up to 270 ℃ of insulation reaction 3 hours then, stop to feed nitrogen; The open vacuum pump was extracted low-boiling point material out with 25 minutes, and logical at last nitrogen is cooled to 220 ℃ of dischargings.
The softening point of product is 97.5 ℃, and Ghana's look 4, acid number are 16.25 (mgKOH/g).
The softening point measurement method adopts ring and ball method, and look level assay method adopts Ghana's colorimetric method for determining by standard GB/T1772-92 regulation.Acid number national standard (GB 1028-88) prescriptive procedure is measured.
Embodiment 6
1, composite catalyst P 2O 5/ SiO 2/ Al 2O 3Preparation
1. used raw material weight proportioning: positive tetraethyl orthosilicate: softex kw: aluminium oxide is 1:0.5:0.3,
2. positive tetraethyl orthosilicate, softex kw, aluminium oxide are joined in the beaker in proportion, using ammoniacal liquor to transfer pH is 9, and normal temperature stirs down and formed colloidal sol in 2 hours; Colloidal sol is moved in the teflon-lined stainless steel reactor; The sealing, in baking oven in 120 ℃, crystallization 48 h; Crystallization is separated the crystalline solid product after finishing with mother liquor, spend deionised water to neutral; At 60 ℃ of drying 12 h, product is 500 ℃ of roasting 3 h in Muffle furnace, binary composite oxides SiO again 2/ Al 2O 3Use 1molL -1Phosphorous acid solution is soaked SiO 2/ Al 2O 324h, suction filtration, 60 ℃ of dry 12h, 450 ℃ of roasting 4h obtain ternary compound oxides P 2O 5/ SiO 2/ Al 2O 3, be composite catalyst of the present invention.
2, the preparation of ester gum
Composite catalyst P with the above-mentioned preparation of 0.16g 2O 5/ SiO 2/ Al 2O 3Join in the four-hole boiling flask of the 250ml of having thermometer, mechanical agitator, nitrogen breather pipe and condenser pipe with 80g rosin, airtight, vacuumize; Feed nitrogen, vacuumize again, feed nitrogen then as protection gas; Heating rosin starts electric mixer, when temperature is elevated to 180 ℃ after all having fused; Add 9.0ml glycerine, be warmed up to 270 ℃ of insulation reaction 5 hours then, stop to feed nitrogen; The open vacuum pump is with extracting low-boiling point material half an hour out, and logical at last nitrogen is cooled to 220 ℃ of dischargings.
The softening point of product is 97.8 ℃, and Ghana's look 4, acid number are 10.76 (mgKOH/g).
The softening point measurement method adopts ring and ball method, and look level assay method adopts Ghana's colorimetric method for determining by standard GB/T1772-92 regulation.Acid number national standard (GB 1028-88) prescriptive procedure is measured.

Claims (5)

1. composite catalyst is characterized in that: the raw material components and the weight proportion that are used to prepare the composite catalyst of pale rosin glyceride are: positive tetraethyl orthosilicate: softex kw: aluminium oxide=1: 0.3 ~ 0.6: 0.1 ~ 0.3.
2. preparation method who prepares the described composite catalyst of claim 1 is characterized in that:
(1) mixed raw material is equipped with colloidal sol: take by weighing raw material by proportioning, add ammoniacal liquor then and mix adjusting pH to 8 ~ 9; Stir and form colloidal sol;
(2) binary composite oxides preparation: colloidal sol filters through crystallization, washing, and roasting makes the binary composite oxides, and main component is SiO 2And Al 2O 3
(3) ternary compound oxides preparation: the binary composite oxides are through 0.5 ~ 1molL -1Phosphorous acid solution is soaked 24 ~ 36h, suction filtration, and drying obtains the composite catalyst of ternary compound oxides then behind 450 ~ 550 ℃ of following roasting 2 ~ 4h..
3. the preparation method of composite catalyst according to claim 2 is characterized in that: said crystallization is meant and colloidal sol is placed 100 ~ 130 ℃ baking oven crystallization 48 ~ 60 h; Crystalline solid product and the mother liquor isolated by filtration of said filtration after with crystallization; Said washing is that the crystalline solid product is spent deionised water to neutral; Said roasting is meant that the crystalline solid product after the washing obtains the binary composite oxides behind roasting 2 ~ 4 h in rearmounted 450 ~ 600 ℃ of 55 ~ 65 ℃ of down dry 11 ~ 13 h.
4. according to the application of the arbitrary described composite catalyst of claim 1 ~ 3 in preparation pale rosin glyceride, it is characterized in that: rosin and said composite catalyst are placed in the reaction vessel, vacuumized 20 ~ 30 minutes; Feed nitrogen as protective gas, be heated to rosin all after the fusion, stir; When temperature is increased to 170 ~ 190 ℃, add glycerine, be warmed up to 260 ~ 280 ℃ then; Insulation reaction 3 ~ 5 hours; Start vavuum pump and extract low-boiling-point substance out, be cooled to 210 ~ 230 ℃ of dischargings then, obtain pale rosin glyceride.
5. the application of composite catalyst according to claim 4 in preparation pale rosin glyceride, it is characterized in that: the weight ratio of said rosin and composite catalyst is 1: 0.001 ~ 0.005, the weight ratio of rosin and glycerine is 1: 0.1 ~ 0.12.
CN2012100887139A 2012-03-30 2012-03-30 Composite catalyst and application thereof in preparing pale rosin glyceride Expired - Fee Related CN102631940B (en)

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Cited By (4)

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Publication number Priority date Publication date Assignee Title
CN104194635A (en) * 2014-08-07 2014-12-10 广西众昌树脂有限公司 Reduced-color reagent for preparing light-colored glycerol ester of rosin
CN105754485A (en) * 2016-04-15 2016-07-13 梧州市飞卓林产品实业有限公司 Rosin glycerin ester production method
CN105778766A (en) * 2016-04-15 2016-07-20 梧州市飞卓林产品实业有限公司 Preparation method of glycerol ester of rosin
CN115869959A (en) * 2022-10-11 2023-03-31 合肥工业大学 Carbon-supported cerium-doped tin oxide magnetic catalyst, preparation method and application

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CN1077461A (en) * 1993-05-12 1993-10-20 福建省龙岩地区林产工业公司 The manufacture method of light colour modified rosin phenolic aldehyde resin
CN1392099A (en) * 2002-07-30 2003-01-22 复旦大学 SAPO-11 molecualr sieve and its preparing method
CN101264454A (en) * 2008-03-21 2008-09-17 广州英科新材料有限公司 Composite catalyst and its application in preparing light-colored rosin esters
CN101372605A (en) * 2008-10-22 2009-02-25 昆明理工大学 Method for preparing rosin glyceride by microwave irradiation

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1077461A (en) * 1993-05-12 1993-10-20 福建省龙岩地区林产工业公司 The manufacture method of light colour modified rosin phenolic aldehyde resin
CN1392099A (en) * 2002-07-30 2003-01-22 复旦大学 SAPO-11 molecualr sieve and its preparing method
CN101264454A (en) * 2008-03-21 2008-09-17 广州英科新材料有限公司 Composite catalyst and its application in preparing light-colored rosin esters
CN101372605A (en) * 2008-10-22 2009-02-25 昆明理工大学 Method for preparing rosin glyceride by microwave irradiation

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104194635A (en) * 2014-08-07 2014-12-10 广西众昌树脂有限公司 Reduced-color reagent for preparing light-colored glycerol ester of rosin
CN105754485A (en) * 2016-04-15 2016-07-13 梧州市飞卓林产品实业有限公司 Rosin glycerin ester production method
CN105778766A (en) * 2016-04-15 2016-07-20 梧州市飞卓林产品实业有限公司 Preparation method of glycerol ester of rosin
CN105754485B (en) * 2016-04-15 2018-07-31 梧州市飞卓林产品实业有限公司 The production method of rosin glycerides
CN115869959A (en) * 2022-10-11 2023-03-31 合肥工业大学 Carbon-supported cerium-doped tin oxide magnetic catalyst, preparation method and application

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