CN110028659A - A kind of synthesis technology of ordor removing quick-drying alkide resin - Google Patents
A kind of synthesis technology of ordor removing quick-drying alkide resin Download PDFInfo
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- CN110028659A CN110028659A CN201910318055.XA CN201910318055A CN110028659A CN 110028659 A CN110028659 A CN 110028659A CN 201910318055 A CN201910318055 A CN 201910318055A CN 110028659 A CN110028659 A CN 110028659A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/66—Polyesters containing oxygen in the form of ether groups
- C08G63/668—Polyesters containing oxygen in the form of ether groups derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/676—Polyesters containing oxygen in the form of ether groups derived from polycarboxylic acids and polyhydroxy compounds in which at least one of the two components contains aliphatic unsaturation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/78—Preparation processes
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D167/00—Coating compositions based on polyesters obtained by reactions forming a carboxylic ester link in the main chain; Coating compositions based on derivatives of such polymers
- C09D167/08—Polyesters modified with higher fatty oils or their acids, or with natural resins or resin acids
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- Polymers & Plastics (AREA)
- Oil, Petroleum & Natural Gas (AREA)
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Abstract
The present invention discloses a kind of synthesis technology of ordor removing quick-drying alkide resin, prepare a four-hole boiling flask as reaction vessels, it is firstly added soybean oleic acid, 95% pentaerythrite, auxiliary agent, dimethylbenzene, nitrogen is then passed through to replace inner air, thermometer is inserted into measure reacting liquid temperature, and be packed into condensation and equip so that solvent constantly flows back, during which keep the leakproofness of reaction vessels.The reaction solution in flask is warming up to 215 ± 3 DEG C with heating and stirring device, heat preservation 1-1.5 hours, it is cooled to 120 ± 5 DEG C, diethylene glycol (DEG), neopentyl glycol, glycerol, phthalic enhydride, maleic anhydride, solvent is added, it is warming up to 175 ± 5 DEG C, heat preservation 1-1.5 hours, persistently overheating one hour to 195 ± 3 DEG C again, heat preservation 0.8-1.3 hours, it is warming up to 210 ± 5 DEG C of heat preservations 1.0-1.6 hours again, 120 DEG C are cooled to after being warming up to 220 DEG C of -224 DEG C of esterifications to viscosity, acid value qualification again, solubilizer thinning filtering and discharging.
Description
Technical field
The present invention relates to chemical technology field more particularly to a kind of synthesis technologies of ordor removing quick-drying alkide resin.
Background technique
Alkyd resin mainly do coating, paint, metal protection, furniture, vehicle, in terms of be widely used.
Alkyd resin is with polyalcohol, polyacid through linear polyesters made of fatty acid modified copolycondensation, and molecular structure is with polyalcohol
Ester be main chain, using aliphatic ester as side chain.Alkyd resin can use fatty acid process, fatty acid-oil process, oily dilution method, alcoholysis method
Manufacture.Wherein fatty acid process and alcoholysis method are most important methods.And fatty acid process often does alkyd resin with solwution method.It is former
Reason is reacted in dimethylbenzene equal solvent, and dimethylbenzene is both solvent and azeotrope with water liquid, can be improved reaction rate and
Reaction is generated into water and takes reaction kettle out of, accelerates the progress of reaction.Reaction temperature is low compared with melting polycondensation, and product color is shallow, but uses
The smell that the method synthetic alkyd resin generates is big, pollute environment and the alkyd resin smell of synthesis is larger.
Summary of the invention
Aiming at the problems existing in the prior art, the purpose of the present invention is to provide a kind of conjunctions of ordor removing quick-drying alkide resin
At technique, basically odorless, environment friendly and pollution-free, equipment investment is few, and quality is pure for resin made from the synthetic method, is used for woodenware
When paint and finishing coat, film forming ordor removing effect is good, and solvent volatility can be good, and gloss stability is good, and resistance to scraping is excellent, is able to satisfy suite and wine
The requirement of shop woodwork industry, securely and reliably.
To achieve the above objectives, the present invention adopts the following technical scheme:
A kind of synthesis technology of ordor removing quick-drying alkide resin, which is characterized in that by weight percentage, including following technique
Step:
A, soybean oleic acid, the 10- of 20-25% are sequentially added in the flask that condensing unit, agitating heater are housed at one
16% 95% pentaerythrite, 0.1-0.5% auxiliary agent, 0.8-1.5% dimethylbenzene；
B, the air that is passed through in Xiang Suoshu flask in nitrogen displacement flask, insertion thermometer to measure the temperature of reaction solution in bottle,
The agitating heater is opened, the reaction solution in the flask is heated to 215 ± 3 DEG C, keeps the temperature 1-1.5 hours；
C, 120 ± 5 DEG C are cooled to, the diethylene glycol (DEG), 2-7% neopentyl glycol, 20-27% phthalic anhydride, 0.2- of 2-6% is added
0.5% maleic anhydride, 1.0-2.1% glycerol, 1.8-2.5% dimethylbenzene are warming up to 175 ± 5 DEG C, and heat preservation 0.8-1.3 is small
When, it is gradually warmed up 1 hour to 195 ± 3 DEG C, keeps the temperature 0.8-1.3 hours, then be warming up to 210 ± 5 DEG C, keep the temperature 1-1.6 hours；
D, 120 DEG C or 120 DEG C are cooled to hereinafter, adding 25- again after being warming up to 220-224 DEG C of heat preservation esterification to viscosity, acid value qualification
36% diluted solvent agitation and dilution, filtering and discharging.
As a further illustration of the above scheme, the synthesis technology of the ordor removing quick-drying alkide resin includes following synthesis work
Skill step:
A, one equipped with condensing unit, agitating heater flask in sequentially add 21% soybean oleic acid, 13%
95% pentaerythrite, 0.21% auxiliary agent, 1.14% dimethylbenzene；
B, the air that is passed through in Xiang Suoshu flask in nitrogen displacement flask, insertion thermometer to measure the temperature of reaction solution in bottle,
The agitating heater is opened, the reaction solution in the flask is heated to 215 DEG C, keeps the temperature 1.5 hours；
C, 120 DEG C are cooled to, be added 4% diethylene glycol (DEG), 3.5% neopentyl glycol, 23.4% phthalic anhydride, 0.35% along fourth
Enedioic acid acid anhydride, 1.5% glycerol, 1.9% dimethylbenzene are warming up to 175 DEG C, keep the temperature 1 hour, are gradually warmed up 1 hour to 195 DEG C, protect
Temperature 1 hour, then 210 DEG C are warming up to, keep the temperature 1 hour；
D, 120 DEG C or 120 DEG C are cooled to hereinafter, adding 30% thinning again after being warming up to 222 DEG C of heat preservation esterifications to viscosity, acid value qualification
Stirring solvent dilution, filtering and discharging.
As a further illustration of the above scheme, the auxiliary agent is hypophosphorous acid or antioxidant.
As a further illustration of the above scheme, the diluted solvent is that arene organic solvent or esters are organic molten
Agent.
As a further illustration of the above scheme, the diluted solvent is 93% dimethylbenzene and 7% butyl acetate group
At.
As a further illustration of the above scheme, the synthesis technology of the ordor removing quick-drying alkide resin includes following synthesis work
Skill step:
420g soybean oil is successively added in a 2000ml four-hole boiling flask equipped with agitating device, thermometer and logical nitrogen protection
Acid, 95% pentaerythrite of 260g, 4.2g hypophosphorous acid or antioxidant, 22.8g dimethylbenzene, while installing condenser and thermometer simultaneously
Stirring and heating are started, is warming up to 215 DEG C, keeps the temperature 1.5 hours；
120 DEG C are cooled to, 80g diethylene glycol (DEG), 70g neopentyl glycol, 468g phthalic anhydride, 30g glycerol, 7g are added again along fourth
Enedioic acid acid anhydride, 38g dimethylbenzene, while stirring and heating are started, 175 DEG C are warming up to, 1 hour is kept the temperature；
Persistently overheating 1 hour to 195 DEG C, keeps the temperature 1 hour again；It is warming up to 210 DEG C again, keeps the temperature 1 hour；
It is warming up to 220-224 DEG C again, heat preservation esterification to acid value, viscosity are qualified, are cooled to 120 DEG C or 120 DEG C or less additions
560g dimethylbenzene, 40g butyl acetate, dilution stir evenly, filtering and discharging.
As a further illustration of the above scheme, esterification to qualification of stating is that be esterified to the acidity of the reaction solution be 8-
10mgKOH/g, range of viscosities 15-16s, the viscosity number measure under conditions of 25 DEG C of format pipes.
The beneficial effects of the present invention are:
Basically odorless, environment friendly and pollution-free, equipment investment is few for resin made from technique of the present invention using two step synthetic method,
Quality is pure, and when being used for woodcare paint and finishing coat, film forming ordor removing effect is good, and solvent volatility can be good, and gloss stability is good, resistance to scraping
It is excellent, it is able to satisfy the requirement of suite and hotel furniture manufacturing, securely and reliably.
Specific embodiment
A specific embodiment of the invention is further described below with reference to embodiment, makes technical solution of the present invention
And its benefits are clearer.The embodiments described below is exemplary, it is intended to be explained the present invention, and cannot be managed
Solution is limitation of the present invention.
The purpose of the present invention is to provide a kind of synthesis technologies of ordor removing quick-drying alkide resin, to overcome gas in the prior art
The disadvantages of taste is big, pollutes environment, the soybean oleic acid itself in formula is vegetable oil acid, environment protection health.Below with reference to embodiment and
The present invention is described in detail for comparative example, and the preparation process flow of ordor removing quick-drying alkide resin is following, and (following percentage is should
Material quality accounts for the percentage of total raw material quality):
A, soybean oleic acid, the 10- of 20-25% are sequentially added in the flask that condensing unit, agitating heater are housed at one
16% 95% pentaerythrite, 0.1-0.5% auxiliary agent, 0.8-1.5% dimethylbenzene；
B, the air that is passed through in Xiang Suoshu flask in nitrogen displacement flask, insertion thermometer to measure the temperature of reaction solution in bottle,
The agitating heater is opened, the reaction solution in the flask is heated to 215 ± 3 DEG C, keeps the temperature 1-1.5 hours；
C, 120 ± 5 DEG C are cooled to, the diethylene glycol (DEG), 2-7% neopentyl glycol, 20-27% phthalic anhydride, 0.2- of 2-6% is added
0.5% maleic anhydride, 1.0-2.1% glycerol, 1.8-2.5% dimethylbenzene are warming up to 175 ± 5 DEG C, and heat preservation 0.8-1.3 is small
When, it is gradually warmed up 1 hour to 195 ± 3 DEG C, keeps the temperature 0.8-1.3 hours, then be warming up to 210 ± 5 DEG C, keep the temperature 1-1.6 hours；
D, 120 DEG C or 120 DEG C are cooled to hereinafter, adding 25- again after being warming up to 220-224 DEG C of heat preservation esterification to viscosity, acid value qualification
36% diluted solvent agitation and dilution, filtering and discharging.
Wherein, the preparation process flow of ordor removing quick-drying alkide resin is as follows
A, one equipped with condensing unit, agitating heater flask in sequentially add 21% soybean oleic acid, 13%
95% pentaerythrite, 0.21% auxiliary agent, 1.14% dimethylbenzene；
B, the air that is passed through in Xiang Suoshu flask in nitrogen displacement flask, insertion thermometer to measure the temperature of reaction solution in bottle,
The agitating heater is opened, the reaction solution in the flask is heated to 215 DEG C, keeps the temperature 1.5 hours；
C, 120 DEG C are cooled to, be added 4% diethylene glycol (DEG), 3.5% neopentyl glycol, 23.4% phthalic anhydride, 0.35% along fourth
Enedioic acid acid anhydride, 1.5% glycerol, 1.9% dimethylbenzene are warming up to 175 DEG C, keep the temperature 1 hour, are gradually warmed up 1 hour to 195 DEG C, protect
Temperature 1 hour, then 210 DEG C are warming up to, keep the temperature 1 hour；
D, 120 DEG C or 120 DEG C are cooled to hereinafter, adding 30% thinning again after being warming up to 222 DEG C of heat preservation esterifications to viscosity, acid value qualification
Stirring solvent dilution, filtering and discharging.
The auxiliary agent is hypophosphorous acid or antioxidant；The diluted solvent is that arene organic solvent or esters are organic molten
Agent.
Embodiment 1:
The preparation process flow of ordor removing quick-drying alkide resin is as follows:
Step 1: successively add in a 2000ml four-hole boiling flask equipped with agitating device, thermometer and logical nitrogen protection
Enter 420g soybean oleic acid, 95% pentaerythrite of 260g, 4.2g hypophosphorous acid, 22.8g dimethylbenzene, while installing condenser and temperature
Stirring and heating are counted and started, is warming up to 215 DEG C, keeps the temperature 1.5 hours.
Step 2: being cooled to 120 DEG C, and 80g diethylene glycol (DEG), 70g neopentyl glycol, 468g phthalic anhydride, 30g are added again
Glycerol, 7g maleic anhydride, 38g dimethylbenzene, while stirring and heating are started, 175 DEG C are warming up to, 1 hour is kept the temperature.Again
Persistently overheating 1 hour to 195 DEG C, keeps the temperature 1 hour.
Step 3: being warming up to 210 DEG C again, keeps the temperature 1 hour.
Step 4: it is warming up to 220-224 DEG C again, heat preservation esterification to acid value is 8-10mgKOH/g, range of viscosities
It is 25 DEG C of 15-16s/ lattice, is cooled to 120 DEG C or less.
Step 5: being added 560g dimethylbenzene, 40g butyl acetate, and dilution stirs evenly, filtering and discharging.
According to relevant national standard, the basic performance of ordor removing alkyd resin of the invention is detected, detection data is such as
The following table 1:
Table 1
| Inspection project | Inspection result | Test stone |
| Color (iron cobalt colorimetric) number | 1.0 | GB/T1722-1992 |
| Appearance and transparency | Limpid, transparent inorganic tool impurity | GB/T1721-1979 |
| Fineness μm | 10 | GB/T1724-1989 |
| Viscosity (mpas/25 DEG C) | 31000 | GB/T1723-1993 |
| Solid content % | 64.75 | GB/T1725-1989 |
| Acid value mgKOH/g | 5.82 | HG2-569-1977 |
According to relevant national standard, to ordor removing quick-drying alkide resin of the invention and comparative example (BR283,
Novalkyd3733 its basic performance is detected after) being made into finishing coat respectively, testing result is as shown in table 2 below.
Table 2
According to the ultimate test needs of resin, recommend paint following (by mass percentage) using test formulations: resin:
76%, anti-settling slurry: 2%, EFKA4010 dispersing agent: 1%, butyl acetate: 4.8%, ED-2 flatting silica: 5%, L778 wax powder:
0.5%, BYK-141 defoaming agent: 0.3%, BYK-306 levelling agent: 0.3%, Tego streamer agent: 0.1%, PMA solvent: 10%.
From the test result of table 2 can be seen that finishing coat smell that ordor removing quick-drying alkide resin prepared by the present invention is matched compared with
Low, hardness richness is good, occupies certain advantage, and other performance is also suitable.
From the foregoing description of structures and principles it should be understood by those skilled in the art that, the present invention not office
It is limited to above-mentioned specific embodiment, this hair is all fallen within using the improvement of techniques well known and substitution on the basis of the present invention
Bright protection scope, protection scope of the present invention should limit it by each claim and its equivalent.In specific embodiment
The part not illustrated is the prior art or common knowledge.
Claims (6)
1. a kind of synthesis technology of ordor removing quick-drying alkide resin, which is characterized in that by mass percentage, including following synthesis work
Skill step:
A, soybean oleic acid, the 10- of 20-25% are sequentially added in the flask that condensing unit, agitating heater are housed at one
16% 95% pentaerythrite, 0.1-0.5% auxiliary agent, 0.8-1.5% dimethylbenzene；
B, the air that is passed through in Xiang Suoshu flask in nitrogen displacement flask, insertion thermometer to measure the temperature of reaction solution in bottle,
The agitating heater is opened, the reaction solution in the flask is heated to 215 ± 3 DEG C, keeps the temperature 1-1.5 hours；
C, 120 ± 5 DEG C are cooled to, the diethylene glycol (DEG), 2-7% neopentyl glycol, 20-27% phthalic anhydride, 0.2- of 2-6% is added
0.5% maleic anhydride, 1.0-2.1% glycerol, 1.8-2.5% dimethylbenzene are warming up to 175 ± 5 DEG C, and heat preservation 0.8-1.3 is small
When, it is gradually warmed up 1 hour to 195 ± 3 DEG C, keeps the temperature 0.8-1.3 hours, then be warming up to 210 ± 5 DEG C, keep the temperature 1-1.6 hours；
D, 120 DEG C or 120 DEG C are cooled to hereinafter, adding 25- again after being warming up to 220-224 DEG C of heat preservation esterification to viscosity, acid value qualification
36% diluted solvent agitation and dilution, filtering and discharging.
2. the synthesis technology of ordor removing quick-drying alkide resin according to claim 1, which is characterized in that the ordor removing quick-drying alcohol
The synthesis technology of acid resin includes following synthesis technology step:
A, one equipped with condensing unit, agitating heater flask in sequentially add 21% soybean oleic acid, 13%
95% pentaerythrite, 0.21% auxiliary agent, 1.14% dimethylbenzene；
B, the air that is passed through in Xiang Suoshu flask in nitrogen displacement flask, insertion thermometer to measure the temperature of reaction solution in bottle,
The agitating heater is opened, the reaction solution in the flask is heated to 215 DEG C, keeps the temperature 1.5 hours；
C, 120 DEG C are cooled to, be added 4% diethylene glycol (DEG), 3.5% neopentyl glycol, 23.4% phthalic anhydride, 0.35% along fourth
Enedioic acid acid anhydride, 1.5% glycerol, 1.9% dimethylbenzene are warming up to 175 DEG C, keep the temperature 1 hour, are gradually warmed up 1 hour to 195 DEG C, protect
Temperature 1 hour, then 210 DEG C are warming up to, keep the temperature 1 hour；
D, 120 DEG C or 120 DEG C are cooled to hereinafter, adding 30% thinning again after being warming up to 222 DEG C of heat preservation esterifications to viscosity, acid value qualification
Stirring solvent dilution, filtering and discharging.
3. the synthesis technology of ordor removing quick-drying alkide resin according to claim 1 or 2, which is characterized in that the auxiliary agent is
Hypophosphorous acid or antioxidant.
4. the synthesis technology of ordor removing quick-drying alkide resin according to claim 1 or 2, which is characterized in that the thinning is molten
Agent is arene organic solvent or based organic solvent.
5. according to claim 1 or the synthesis technology of 2 any ordor removing quick-drying alkide resins, which is characterized in that described to convert
Dilute solvent is made of 93% dimethylbenzene and 7% butyl acetate.
6. the synthesis technology of ordor removing quick-drying alkide resin according to claim 1 or 2, which is characterized in that the esterification is extremely
Qualification be esterification to the reaction solution acidity be 8-10mgKOH/g, range of viscosities 15-16s, the viscosity number is at 25 DEG C
It is measured under conditions of format pipe.
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| CN201910318055.XA CN110028659A (en) | 2019-04-19 | 2019-04-19 | A kind of synthesis technology of ordor removing quick-drying alkide resin |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115449063A (en) * | 2022-10-24 | 2022-12-09 | 昆勒聚合物(上海)有限公司 | Low-odor high-hardness high-sealing-performance woodware sealing primer polymer |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105399934A (en) * | 2015-11-13 | 2016-03-16 | 惠州市长润发涂料有限公司 | Process for synthesizing low-odor alkyd resin by adopting two-step method |
| CN109575255A (en) * | 2018-11-22 | 2019-04-05 | 三棵树涂料股份有限公司 | A kind of preparation method of ordor removing quick-drying alkide resin |
-
2019
- 2019-04-19 CN CN201910318055.XA patent/CN110028659A/en not_active Withdrawn
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105399934A (en) * | 2015-11-13 | 2016-03-16 | 惠州市长润发涂料有限公司 | Process for synthesizing low-odor alkyd resin by adopting two-step method |
| CN109575255A (en) * | 2018-11-22 | 2019-04-05 | 三棵树涂料股份有限公司 | A kind of preparation method of ordor removing quick-drying alkide resin |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115449063A (en) * | 2022-10-24 | 2022-12-09 | 昆勒聚合物(上海)有限公司 | Low-odor high-hardness high-sealing-performance woodware sealing primer polymer |
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Application publication date: 20190719 |