CN102337078A - Production process for rosin resin - Google Patents
Production process for rosin resin Download PDFInfo
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- CN102337078A CN102337078A CN2011101892981A CN201110189298A CN102337078A CN 102337078 A CN102337078 A CN 102337078A CN 2011101892981 A CN2011101892981 A CN 2011101892981A CN 201110189298 A CN201110189298 A CN 201110189298A CN 102337078 A CN102337078 A CN 102337078A
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Abstract
The invention provides a method of preparing rosin ester or modified rosin ester from rosin. The method comprises a preparation step and an esterification step for modified rosin. The invention is characterized by further comprising a refining process for rosin carried out before the esterification step for modified rosin, and the refining process comprises a step of distillation. According to the step of distillation, rosin is placed into a distilling still and heated under vacuum, distilled fractions boiling in a range of 180 to 220 DEG C are collected separately, then main fractions are collected, and refined rosin is obtained after the temperature of rosin reaches 270 DEG C.
Description
Technical field
The present invention relates to a kind ofly prepare the method for rosin derivative, especially a kind of method for preparing rosin ester by rosin by rosin.
Background technology
The rosiny staple is a resinous acid, and there are two reactive groups in resinous acid: two two keys (perhaps more active conjugated double bond) and a carboxyl.Through being carried out the resulting product of chemical reaction with unsaturated compound (like toxilic acid, vinylformic acid an etc.) Diels-Alder, two keys (or conjugated double bond) are commonly referred to modified rosin; And carboxyl is commonly referred to rosin derivative as the resulting product of reactive group, all modified rosins also can utilize its carboxyl that stays to make various verivates.Modified rosin mainly contains staybelite, nilox resin, polymerized rosin and maleated rosin, and rosin derivative mainly contains rosin ester class, rosin salt, rosin nitrile and rosin Amine D etc.Wherein maleated rosin as the reinforcement sizing agent on the process industry, also is coating, printing ink, tackiness agent mainly, the main raw material of industry such as viton.Its working method mainly contains two kinds of solvent method and scorifications.
Provide a kind of toxilic acid glycerin abietate modified preparation method among the CN1085929A, wherein used basic metal or alkaline earth metal oxide and its esters to come the color of aufhellung product and increase the yield of product as catalyzer.A kind of catalytic esterification rosin method is provided among the CN1208061A, and catalyst system therefor is the tin alkyl acids.A kind of method of synthesizing maleated rosin rapidly is provided among the CN1872929A, and what it adopted is the sonochemistry method.A kind of preparation method of HV low softening point Gum Rosin is provided among the CN101649161A.A kind of method of utilizing fumaric acid to produce high-softening-point rosin glyceride then is provided among the CN101818027A.
But in the above-mentioned technology, raw material rosiny purity is lower, perhaps complicated process of preparation, thus make the quality product of rosin ester or modified rosin ester not reach requirement, can't really realize industrialization.
Summary of the invention
For overcoming above-mentioned defective, the present invention provides a kind of method that is prepared rosin ester by rosin.
The present invention realizes through following technical scheme:
A kind ofly prepare the method for rosin ester, it is characterized in that, before the rosiny esterif iotacation step, also comprise a rosiny treating process by rosin.
According to the present invention, described preparation method also comprises rosin is carried out modification.The preferred polyprotonic acid that adopts carries out modification.
According to optimal technical scheme of the present invention, said polyprotonic acid is preferably fumaric acid or toxilic acid, more preferably toxilic acid.The temperature of said modifying process is controlled at about 200 ℃.The time of said modifying process is approximately 6 hours.
According to the present invention, said preparation method also comprises the rosiny esterification process.Said step preferably includes: will change esterifying kettle over to through the resin of metering, and add oxidation inhibitor and polyvalent alcohol and carry out esterification, and carry out aftertreatment after esterification is accomplished and get the rosin ester finished product.
According to optimal technical scheme of the present invention, also comprise modifying process before the said rosiny esterification process.
Preferred concrete technology is following:
(4) rosiny is refining;
(5) rosiny modification is characterized in that, will change esterifying kettle over to through the resin of metering, adds polyprotonic acid and carries out modification;
(6) rosiny esterification is characterized in that, the rosin after the modification is added polyvalent alcohol carry out esterification, preferably adds inhibitor.
According to the present invention, the polyvalent alcohol that adopts in the said esterification process is preferably glycerine.
According to the present invention, the temperature of said esterification process is controlled between 240-270 ℃.Too low like temperature, then the speed of esterification is too slow, causes esterification incomplete, influences product acid value and softening temperature, and is too high like esterification temperature, is prone to cause polyvalent alcohol cracking and rosin cracking, goes out waste product.
According to the present invention, said method is carried out aftertreatment after also being included in esterification.
According to optimal technical scheme of the present invention, the aftertreatment after the said esterification comprises feeding steam and/or vacuumizes.
According to the present invention, said rosiny purification step comprises a distilation steps, is about to rosin and adds in the still kettle, under vacuum, heat, wherein 180-220 ℃ distillate the part single collection, carry out the collection of main fraction then.
According to the present invention, said process for purification comprises the part that distillates after collecting 240 ℃.Cut within preferably collecting 270 ℃.
According to the present invention, the distillation temperature of the main fraction of said treating process need be controlled within 270 ℃, like the too high rosin Pintsch process that then causes easily of temperature, has a strong impact on resin color and softening temperature.
According to the present invention, said treating process specifically comprises:
(1) rosin is pressed into the rosin test tank with nitrogen from the rosin basin, changes still kettle after metering over to, open deep fat the still kettle material is heated up;
(2) and the open vacuum unit, distill out the part single collection behind the foreshot basin with 180-220 ℃, pipeline is switched to main fraction basin begin to carry out main fraction and collect;
(3) reach 270 ℃ to temperature of charge, and observe from visor and to close deep fat when no rosin distillates, close the vacuum unit, nitrogen replacement is gone into still kettle and reception still, make resin.
According to the present invention, it is residual that the remainder in still kettle is still, but sell after the barrelling.
According to the present invention, said treating process need keep the reactive system resistance to air loss, and promptly reactive system requires high-air-tightness, and not high like resistance to air loss, air admission then is prone to cause the product oxidation, has a strong impact on product colour.
According to the present invention, described concrete preparation technology is following:
1, rosin rectification flow
Rosin is pressed into the rosin test tank with nitrogen from the rosin dissolution kettle; Change still kettle after metering over to, open deep fat the still kettle material is heated up, and the open vacuum unit; Distill out the part single collection behind the foreshot basin with 180-220 ℃; Pipeline is switched to main fraction basin begin to carry out main fraction and collect, reach 270 ℃ to temperature of charge, and observe from visor and to close deep fat when no rosin distillates, close the vacuum unit; Nitrogen replacement is gone into still kettle and main distillate fraction basin, change the resin that makes over to esterifying kettle and carry out further deep processing.
Simultaneously, it is residual that the remainder in the still kettle is still, sells after the barrelling.
2, rosin esterification flow process
To change esterifying kettle over to through the resin of metering, and add polyprotonic acid and about 200 ℃, carry out modification, add oxidation inhibitor and glycerine after modification is accomplished at 230 ℃-270 ℃; Preferred 240 ℃-260 ℃ are carried out esterification, and said glycerine is stored in the glycerine basin, sends into the glycerine volume pump through the glycerine toothed gear pump and measures; Change esterifying kettle then over to, after 6 hours, lead to steam, vacuumize; Cool to 200 ℃, add the later stage auxiliary material, change product storage tank over to after stirring.
3, finished product packing
With spiral pump the rosin ester in the finished product basin is squeezed into tablets press continuously, after the granulation and cooling through tablets press, it is granular to become the semicircle sphere, in the Gum Rosin lift is promoted to the product storage tank, for sale by becoming the product pile after sacker's pack.
According to optimal technical scheme of the present invention, the name that said rosin treating process preferably adopts the applicant to submit on June 7th, 2011 is called the patented claim of " a kind of rosin refining kettle ", and it introduces this paper as a reference in full.
According to optimal technical scheme of the present invention, said refining kettle comprises round shape pot body, and upper cover and lower cover is characterized in that, this refining kettle comprises the mosquito-repellent incense coil pipe, and said mosquito-repellent incense coil pipe is installed in the lower cover.
According to the present invention, said mosquito-repellent incense coil pipe is near the bottom of pot body.Preferably, said mosquito-repellent incense coil pipe is apart from lower cover valley inwall 300-400mm, preferred 320-350mm.
According to the present invention, said refining kettle also comprises the heating sinuous coil.Said sinuous coil is installed in the lower cover, preferably near the bottom of a pan, and more preferably apart from lower cover valley inwall 120-200mm, preferred 150-180mm.
According to the present invention, said refining kettle also further comprises outer semicircle heating coil.
According to the present invention, said outer semicircle heating coil is arranged on pot body bottom and the lower cover.Preferably, said outer semicircle heating tube is 300-400mm apart from lower cover valley inside wall height on the pot body, preferred 320-350mm.
According to the present invention, said upper cover is taper.Cone angle is 100-150 °, preferred 120 °, is connected with round shape pot body.Said lower cover is oval, is positioned at the bottom of pot body.
According to the present invention, said upper cover is provided with the rosin opening for feed, is used to connect the steam outlet of condensing surface.Said upper cover also further comprises the temp probe installing port.
According to the present invention, said lower cover is oval lower cover.
According to the present invention, said refining kettle bottom also is provided with residual drain hole of still and the residual baiting valve of still.Residual drain hole of said still and the residual baiting valve of still are located at the lower cover valley, in order to will distill residual all the putting totally of the remaining still in end back.The residual refining kettle defective material that is of wherein said still.
According to the present invention, said heating sinuous coil and mosquito-repellent incense coil pipe can be for a plurality of, as 2 or 3.Thereby form heating sinuous coil group and mosquito-repellent incense coil pipe group respectively.
According to the present invention, said sinuous coil and mosquito-repellent incense coil pipe all support with the coil pipe frame.
According to the present invention, said sinuous coil comprises fuel charging valve and delivery valve.Said mosquito-repellent incense coil pipe comprises fuel charging valve and delivery valve.Said outer semicircle coil pipe comprises fuel charging valve and delivery valve.
According to optimal technical scheme of the present invention, said refining kettle comprises sinuous coil, mosquito-repellent incense coil pipe and outer semicircle coil pipe.The preferred technical scheme according to the present invention, said sinuous coil, mosquito-repellent incense coil pipe and outer semicircle coil pipe are opened simultaneously, preferably open each coil pipe oil-feed and fuel-displaced valve simultaneously.
According to the present invention, said sinuous coil, mosquito-repellent incense coil pipe and outer semicircle coil pipe three cover heating coils all are to be used for heating.The purpose that three cover coil pipes are set is: (1) is in order to strengthen heating-surface area; (2) for through the high-order layout of three cover coil pipes, make the rosiny type of heating more flexible.When the rosin liquid level is high, preferably three cover coil pipes are all opened the souping up heating; And after the rosin liquid level descends, just can heat by furnishing two cover coil pipes (preferred mosquito-repellent incense coil pipe and outer semicircle coil pipe); When the rosin liquid level is very low, then can only open the mosquito-repellent incense coil pipe.When the rosin liquid potential drop is low, close sinuous coil fuel charging valve and delivery valve, stop the circulation of high temperature heat conductive oil in sinuous coil, to reduce rosiny cracking and charing phenomenon.
According to the present invention, said process for purification also is included under the few situation of the interior rosin of refining kettle, closes sinuous coil fuel charging valve and delivery valve, stops the circulation of high temperature heat conductive oil in sinuous coil, to reduce rosiny cracking and charing phenomenon.
According to the present invention, said process for purification also further comprises, after the rosin liquid level descends, adopts two cover coil pipe heating, preferably adopts mosquito-repellent incense coil pipe and outer semicircle coil pipe heating, and closes sinuous coil.And when the rosin liquid level is very low, then only open the heating of mosquito-repellent incense coil pipe.
According to the present invention, said refining kettle also comprises temp probe, and this temp probe is arranged on the taper upper cover, be used for surveying showing the rosin temperature, and in order to material temperature in the monitoring refining kettle.
According to the present invention, for guaranteeing rosin purification efficiency and refined prod quality, refining kettle cylindrical shell aspect ratio (height and diameter ratio) is 0.5-1, is preferably 0.6-0.8, more preferably 0.7-0.75.
According to the present invention, said process for purification also comprises temperature of charge in the employing temp probe monitoring refining kettle.
According to the present invention, show the rosiny liquid level through temp probe.Because rosiny viscosity is very big, the rosin viscosity that method especially of the present invention obtains is bigger, and adopts the instrument of common survey liquid level all can't detect.Therefore the present invention infers the rosin liquid level indirectly by means of the rosin temp probe.When the steam state rosin temperature that monitors when the temp probe of finding to be arranged on condensing surface steam state rosin ingress descends rapidly, explain that rosin is few.At this moment, therefore the rosiny liquid level can finish to make with extra care basically in mosquito-repellent incense coil pipe position basically.
Rosin refining kettle of the present invention owing to adopted the taper upper cover, has not only reduced the invalid volume of refining kettle, also because of its bell-mouthed shape, makes the flow velocity quickening at the steam outlet place of steam state rosin, has reduced the rosin backflow, and the burden of vacuum pump group is reduced greatly.
The structure of the sinuous coil among the present invention, mosquito-repellent incense coil pipe and outer semicircle coil pipe is the conventional structure of this area; And rosin refining kettle of the present invention; Just because of having adopted sinuous coil, mosquito-repellent incense coil pipe and outer semicircle coil pipe three cover heating coils; Strengthened the rosin heating-surface area greatly; Can effectively control refining kettle cylindrical shell aspect ratio and rosin is heated evenly, avoid rosin because of local superheating or the not enough rosin that causes of local heating is refining not exclusively, the phenomenon of rosin cracking, rosin charing, improve the yield and the quality product of resin.
In addition; Through the reasonable disposition of three cover coil pipe positions, can also be according to the height of rosin liquid level in treating process, open or the oil inlet and outlet of closed portion coil pipe; Cut off the circulation of thermal oil in this coil pipe; Reach and add thermal control more accurately, thereby make the rosiny utilization ratio increase greatly, avoided because made from extra care the waste that residue rosin causes.
Adopt preparation method of the present invention, the rosin in rosin ester that obtains or the modified rosin ester product reaches national superfine rosin standards.Because national standard is close with it rank standard not, so the applicant generally adopts its product quality of index expression of Gum Rosin.Adopt process for purification of the present invention, the color that obtains the rosin product adopts iron cobalt color ratio color method to detect, and can reach between the 1-2 look.And superfine rosin is with iron cobalt colourimetry, and color is between the 6-7 look, and look is number low more, and grade is high more, and therefore the product that obtains of method of the present invention is far superior to superfine rosin.
According to the present invention, prepared rosin ester or modified rosin ester product can be processed into product through ordinary method as required.For example: with spiral pump the modified rosin resin that makes is squeezed into tablets press continuously, after the granulation and cooling through tablets press, it is granular to process the semicircle sphere, in the Gum Rosin lift is promoted to the product storage tank, by becoming product after sacker's pack.
Description of drawings
Fig. 1: the structural representation for preparing modified rosin ester by rosin of the present invention.
Fig. 2: the structural representation of rosin refining kettle of the present invention.
The implication of each Reference numeral is following:
1: the rosin test tank; 2: still kettle; 3: the front-end volatiles basin; 4: the main distillate fraction basin; 5: refining main condenser; 6: shell-and tube condenser; 7: the glycerine test tank; 8: esterifying kettle; 9: product storage tank; 10: the rosin dissolution kettle; 11: horizontal condenser; 12: vertical (type) condenser; 13: the profit basin; 14: receiver; 15: vacuum buffer tank; 16: vacuum pump; 17: the vacuum unit; 18: spiral cooler; 19: the glycerine basin; 20: the glycerine toothed gear pump.
Wherein the principle of work of condensing surface is to adopt the water coolant of interlayer, utilizes temperature head transmission; Make gaseous state become liquid state.Simultaneously, receiver 14 is used to store the mixture of waste water and oil.
21. the pot body, 22. temp probe mouths, 23. steam outlets, 24. opening for feeds, 25. taper upper covers; 26. the ear seat, 27. sinuous coil oil outlets, 28. mosquito-repellent incense coil pipe oil outlets, 29. outer semicircle coil pipe oil outlets, 30. sinuous coils; 31. oval lower cover, 32. outer semicircle coil pipe oil-ins, 33. mosquito-repellent incense coil pipe oil-ins, the residual baiting valve of 34. stills, the residual drain hole of 35. stills; 36. the sinuous coil oil-in, 37. outer semicircle coil pipes, 38. mosquito-repellent incense coil pipes, 39. coil pipe supports.
Embodiment
The present invention describes the method for preparing modified rosin ester by rosin of the present invention through following embodiment.But those skilled in the art understand, any improvement that the present invention is made or change all within protection scope of the present invention.
Embodiment 1: the method that is prepared the fumaric acid modified ester gum below in conjunction with Fig. 1 explanation by rosin.
1, rosin rectification flow
Rosin is pressed into rosin test tank 1 with nitrogen from rosin dissolution kettle 10, changes still kettle 2 after metering over to, open deep fat the still kettle material is heated up; And the open vacuum unit, distill out the part single collection behind foreshot basin 3 with 180-220 ℃, pipeline is switched to main fraction basin 4 begin to carry out main fraction and collect; Reach 270 ℃ to temperature of charge; And when the no rosin of visor observation distillates, close deep fat, close the vacuum unit, nitrogen replacement is gone into still kettle 2 and received still, change the resin that makes over to esterifying kettle and carry out further deep processing; It is residual that remainder is still in the still kettle, sells after the barrelling.
After making with extra care, obtain the rosin grade and reach national superfine standard.
2, rosin esterification flow process
To change esterifying kettle 8 over to through the resin of metering, and add fumaric acid and carry out modification at 200 ℃; Adding oxidation inhibitor and glycerine carried out esterification at 240 ℃ after modification was accomplished, and said glycerine is stored in the glycerine basin 19, sends into the glycerine volume pump through glycerine toothed gear pump 20 and measures; Change esterifying kettle then over to after 8,6 hours, lead to steam, vacuumize; Cool to 200 ℃, add the later stage auxiliary material, change product storage tank 9 after stirring over to.
3, finished product packing
With spiral pump the rosin ester in the finished product basin 9 is squeezed into tablets press continuously, after the granulation and cooling through tablets press, it is granular to become the semicircle sphere, in the Gum Rosin lift is promoted to the product storage tank, for sale by becoming the product pile after sacker's pack.
The fumaric acid modified ester gum that this embodiment obtains, iron cobalt method detect color less than 1#, and productive rate is greater than 85%.
Embodiment 2: prepare the glycerin abietate modified method of toxilic acid below in conjunction with Fig. 1 explanation by rosin.
Adopt rosin rectification flow (the step 1) acquisition resin among the embodiment 1.
To change esterifying kettle over to through the resin of metering, and add toxilic acid and carry out modification at 200 ℃; Adding oxidation inhibitor and glycerine carried out esterification at 270 ℃ after modification was accomplished, and after 6 hours, led to steam, vacuumized; Cool to 240 ℃, add the later stage auxiliary material, change the storage of finished products groove after stirring over to.
With spiral pump the Gum Rosin in the finished product basin is squeezed into tablets press continuously, after the granulation and cooling through tablets press, it is granular to become the semicircle sphere, in the Gum Rosin lift is promoted to the product storage tank, for sale by becoming the product pile after sacker's pack.
The Malaysia that this embodiment obtains is glycerin abietate modified, and iron cobalt method detects color smaller or equal to 2#, and productive rate is near 100%.
Claims (9)
1. one kind prepares the method for rosin ester by rosin, it is characterized in that, before the rosiny esterif iotacation step, also comprises a rosiny treating process.
2. according to the method for claim 1, it is characterized in that described preparation method also comprises rosin is carried out modification.The preferred polyprotonic acid that adopts carries out modification.Said polyprotonic acid is preferably fumaric acid or toxilic acid, more preferably toxilic acid.
3. according to the method for claim 1 or 2, said preparation method also comprises the rosiny esterification process.Said esterif iotacation step preferably includes: will change esterifying kettle over to through the resin of metering, and add oxidation inhibitor and polyvalent alcohol and carry out esterification, and carry out aftertreatment after esterification is accomplished and get the rosin ester finished product.
4. according to each method of claim 1-3, said modification procedure is before said esterif iotacation step, after purification step.
5. according to the method for claim 4, said technology comprises the steps:
(1) rosiny is refining;
(2) rosiny modification is characterized in that, will change esterifying kettle over to through the resin of metering, adds polyprotonic acid and carries out modification;
(3) rosiny esterification is characterized in that, the rosin after the modification is added polyvalent alcohol carry out esterification, preferably adds inhibitor.
6. according to each method of claim 1-5, it is characterized in that the polyvalent alcohol that adopts in the said esterification process is a glycerine.The temperature of preferred said esterification process is controlled between 240-270 ℃.。
7. according to each method of claim 1-6, it is characterized in that said process for purification comprises the part that distillates after collecting 240 ℃.Cut within preferably collecting 270 ℃.
8. according to each method of claim 1-7, it is characterized in that said purification step comprises as follows:
(1) rosin is pressed into the rosin test tank with nitrogen from the rosin basin, changes still kettle after metering over to, open deep fat the still kettle material is heated up;
(2) and the open vacuum unit, distill out the part single collection behind the foreshot basin with 180-220 ℃, pipeline is switched to main fraction basin begin to carry out main fraction and collect;
(3) reach 270 ℃ to temperature of charge, and observe from visor and to close deep fat when no rosin distillates, close the vacuum unit, nitrogen replacement is gone into still kettle and reception still, make resin.。
9. according to each method of claim 1-8, it is characterized in that said making with extra care in the rosin refining kettle carried out, said refining kettle comprises round shape pot body, upper cover and lower cover and mosquito-repellent incense coil pipe.Preferably, said refining kettle also comprises the heating sinuous coil.More preferably, said refining kettle also further comprises outer semicircle heating coil.
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| CN103436174A (en) * | 2013-08-27 | 2013-12-11 | 广西梧州松脂股份有限公司 | Preparation method of rosin glycerin ester |
| CN104147991A (en) * | 2014-08-07 | 2014-11-19 | 广西众昌树脂有限公司 | Pre-reactor |
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| CN104559793A (en) * | 2013-12-07 | 2015-04-29 | 广西梧州日成林产化工股份有限公司 | High-vacuum continuous distillation production method of light-colored rosin |
| CN105086832A (en) * | 2015-09-29 | 2015-11-25 | 广西梧州日成林产化工股份有限公司 | Rosin distillation method |
| CN105482713A (en) * | 2015-12-25 | 2016-04-13 | 广东科茂林产化工股份有限公司 | Highly-disproportionated rosin glycidyl methacrylate and preparation method thereof |
| CN105802502A (en) * | 2016-04-15 | 2016-07-27 | 梧州市飞卓林产品实业有限公司 | Maleic glyceride preparing method |
| CN106519986A (en) * | 2016-09-23 | 2017-03-22 | 广东科茂林产化工股份有限公司 | Tackifying resin prepared from rosinol recovery material and preparation method thereof |
| CN106928853A (en) * | 2017-04-27 | 2017-07-07 | 德庆明亮树脂有限公司 | A kind of production method of water-white tackifying resins |
| CN107573849A (en) * | 2017-09-18 | 2018-01-12 | 广西众昌树脂有限公司 | The production method of rosin ethylene glycol ester |
| CN110760266A (en) * | 2019-08-12 | 2020-02-07 | 德庆华彩合成树脂有限公司 | Water-soluble fumaric acid modified rosin resin and preparation method thereof |
| US11905438B2 (en) | 2018-06-22 | 2024-02-20 | 3M Innovative Properties Company | Process of manufacturing a pressure sensitive adhesive having a low VOC characteristics |
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