CN110330610A - A kind of synthesis technology of p tert butylphenol formaldehyde resin - Google Patents
A kind of synthesis technology of p tert butylphenol formaldehyde resin Download PDFInfo
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- CN110330610A CN110330610A CN201910648203.4A CN201910648203A CN110330610A CN 110330610 A CN110330610 A CN 110330610A CN 201910648203 A CN201910648203 A CN 201910648203A CN 110330610 A CN110330610 A CN 110330610A
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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
- C08G8/00—Condensation polymers of aldehydes or ketones with phenols only
- C08G8/04—Condensation polymers of aldehydes or ketones with phenols only of aldehydes
- C08G8/08—Condensation polymers of aldehydes or ketones with phenols only of aldehydes of formaldehyde, e.g. of formaldehyde formed in situ
- C08G8/12—Condensation polymers of aldehydes or ketones with phenols only of aldehydes of formaldehyde, e.g. of formaldehyde formed in situ with monohydric phenols having only one hydrocarbon substituent ortho on para to the OH group, e.g. p-tert.-butyl phenol
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Abstract
The invention belongs to disclose a kind of synthesis technology of p tert butylphenol formaldehyde resin to 2-methyl-2-phenylpropane fluosite synthesis technical field.Formalin, ammonium hydroxide are added in reaction kettle；Then it is uniformly added into p-tert-butylphenol, is warming up to boiling later, and is kept for 150-180 minutes；Cooling is added in acetic acid and stirs, and toluene is added and is extracted；After being then allowed to stand layering, waste water is discharged；Oxalic acid, tap water is added waste water is discharged after stirring after stratification；PH ≈ 7-7.5 is detected, normal pressure desolventizing toluene vacuumizes, vacuum pumping blowing, obtains t-Butylphenol formaldehyde resin.The technique is since ammonium hydroxide belongs to weak base, so reaction relatively mitigates, using p tert butylphenol formaldehyde resin made from this method, product index is stablized, and service performance is stablized.
Description
Technical field
The invention belongs to p tert butylphenol formaldehyde resin technical fields, concretely disclose a kind of p-tert-butylphenol
The synthesis technology of formaldehyde resin.
Background technique
Impurity content decides that the quality of p tert butylphenol formaldehyde resin, its fewer performance of impurity content are more stable, outer
It is higher to see transparency.
Currently, the synthesis of p tert butylphenol formaldehyde resin is all made of sodium hydroxide or calcium hydroxide makees catalyst, in life
The washing that 3-5 times is had to pass through during producing, can just obtain the p tert butylphenol formaldehyde resin product of appearance transparent；In addition,
Sodium hydroxide or calcium hydroxide both catalyst belong to strong alkali catalyst, and reaction is relatively acutely, generated to uncle
The molecular weight distribution of butylphenol formaldehyde resin is wide, the stability of product downstream is deteriorated.
" contemporary chemical industry periodical " the 1st phase of volume 31 describes a kind of synthesis side of novel p tert butylphenol formaldehyde resin
Method, this method use calcium hydroxide and 201#Co-catalyst makees catalyst, although raw relative to using sodium hydroxide to make catalyst
For the technique for producing p tert butylphenol formaldehyde resin, washing times are reduced, and the production cycle shortens, but this method equally exists by force
Base catalyzed reactions are violent, the problem of product stability difference, while at the appearance of the p tert butylphenol formaldehyde resin product of output
In translucent, poor transparency.
Summary of the invention
The good p-tert-butylphenol formaldehyde tree of bright and quality stability the object of the present invention is to provide a kind of product appearance
The synthesis technology of rouge.
Realize technical solution used by above-mentioned purpose of the present invention are as follows:
A kind of synthesis technology of p tert butylphenol formaldehyde resin, comprising the following steps:
Stirring is opened, under normal pressure puts into formalin in reaction kettle, then ammonium hydroxide is added in reaction kettle；Then in 50-
At a temperature of 55 DEG C, it is uniformly added into p-tert-butylphenol in 90-100 minutes, is warming up to boiling later, fluidized state keeps 150-
180 minutes；It is cooled to 60-65 DEG C, acetic acid is added and neutralizes, stirs 5-10 minutes, toluene is added and is extracted；Then stop to stir quiet
After setting layering in 10-20 minutes, it is discharged from reactor bottom valve by the waste water of lower layer；Oxalic acid is added, is then turned on stirring and is added
Tap water stirs 5-10 minutes；Then stop after stirring stands 10-20 minute and be layered, equally from reactor bottom valve by lower layer
Waste water discharge；PH ≈ 7-7.5 is detected, normal pressure desolventizing toluene, temperature recovery is to 140-160 DEG C；Vacuumize-0.080 ----
0.085MPa, vacuum pumping blowing, obtains p tert butylphenol formaldehyde resin.
In the synthesis technology of above-mentioned p tert butylphenol formaldehyde resin,
--- described add is warming up to time of boiling after p-tert-butylphenol and controls at 60-70 minutes；
--- the weight of used each component is divided into:
100 parts by weight of p-tert-butylphenol,
The formalin be 100-120 parts by weight and content be 37%,
The ammonium hydroxide be 8-10 parts by weight and content be 25%,
The acetic acid be 3.5-4.5 parts by weight,
180 parts by weight of toluene,
The industrial ethanedioic acid be 1-2 parts by weight and 99% or more content,
The tap water 70-80 parts by weight.
Present invention solves the technical problem that being the catalyst type by changing traditional p tert butylphenol formaldehyde resin, adopt
Catalyst substitution sodium hydroxide is done with ammonium hydroxide.When ammonium hydroxide makees catalyst, it is not easy due to forming two (hydroxyl benzyl) amine or three (hydroxyl benzyl) amine
It is dissolved in water, it makes resin lose water solubility quickly, so extracting link in toluene, water is particularly easy to separate, and washing is primary
Keep finished appearance transparent；Again since ammonium hydroxide belongs to weak base, reaction process compares mitigation, so manufactured p-tert-butylphenol formaldehyde
Resin index are stablized.
Specific embodiment
Combined with specific embodiments below to the synthetic technology of p tert butylphenol formaldehyde resin provided by the present invention make into
The detailed description of one step.
Embodiment 1
Stirring is opened, the formalin that 100Kg content is 37% is put into reaction kettle under normal pressure, is then by 10Kg content
25% ammonium hydroxide is added in reaction kettle, and then at a temperature of 50-55 DEG C, 100Kg is uniformly added into 100 minutes to tert-butyl benzene
Phenol is warming up to boiling for 60 minutes later, and fluidized state is kept for 150 minutes, is cooled to 60 DEG C, and 4.5Kg acetic acid is added and neutralizes, stirring
5 minutes, 180Kg toluene is added and is extracted, then stops stirring and stand after ten minutes, arranged from reactor bottom valve by waste water
Out, oxalic acid 1.0kg is added, is then turned on stirring and 80Kg tap water is added, stir 5 minutes, then stops stirring and stands after ten minutes,
It is equally discharged from reactor bottom valve by waste water, detects pH ≈ 7-7.5, normal pressure desolventizing, temperature recovery is taken out true to 150 DEG C
Empty extremely -0.080MPa, softening point reach 95-100 DEG C of blowing and obtain p-tert-butylphenol formaldehyde resin.
Embodiment 2
Stirring is opened, the formalin that 110Kg content is 37% is put into reaction kettle under normal pressure, is then by 8Kg content
25% ammonium hydroxide is added in reaction kettle, and then at a temperature of 50-55 DEG C, 100Kg p-tert-butylphenol is uniformly added into 95 minutes,
It is warming up within 70 minutes later boiling, fluidized state is kept for 160 minutes, is cooled to 65 DEG C, and 3.5Kg acetic acid is added and neutralizes, stirring 10
Minute, 180Kg toluene is added and is extracted, then stops stirring standing after 15 minutes, is discharged from reactor bottom valve by waste water,
Addition oxalic acid 1.5kg is then turned on stirring and 70Kg tap water is added, stirs 8 minutes, then stops stirring standing after 12 minutes, together
Waste water is discharged from reactor bottom valve for sample, detect pH ≈ 7-7.5, normal pressure desolventizing, temperature recovery to 145 DEG C, vacuumize-
0.085MPa, softening point reach 95-100 DEG C of blowing and obtain p-tert-butylphenol formaldehyde resin.
Embodiment 3
Stirring is opened, the formalin that 100Kg content is 37% is put into reaction kettle under normal pressure, is then by 9Kg content
25% ammonium hydroxide is added in reaction kettle, and then at a temperature of 50-55 DEG C, 100Kg p-tert-butylphenol is uniformly added into 90 minutes,
It is warming up within 65 minutes later boiling, fluidized state is kept for 160 minutes, is cooled to 62 DEG C, and 4.0Kg acetic acid is added and neutralizes, stirs 5 points
Clock is added 180Kg toluene and is extracted, and then stops stirring and stands after twenty minutes, is discharged, adds from reactor bottom valve by waste water
Enter oxalic acid 2.0kg, be then turned on stirring and 70Kg tap water is added, stir 5 minutes, then stops stirring standing after 16 minutes, equally
Be discharged from reactor bottom valve by waste water, detect pH ≈ 7-7.5, normal pressure desolventizing, temperature recovery to 155 DEG C, vacuumize-
0.083MPa, softening point reach 95-100 DEG C of blowing and obtain p-tert-butylphenol formaldehyde resin.
Embodiment 4
Stirring is opened, the formalin that 115Kg content is 37% is put into reaction kettle under normal pressure, is then by 10Kg content
25% ammonium hydroxide is added in reaction kettle, and then at a temperature of 50-55 DEG C, 100Kg p-tert-butylphenol is uniformly added into 100 minutes,
It is warming up within 65 minutes later boiling, fluidized state is kept for 170 minutes, is cooled to 65 DEG C, and 4.5Kg acetic acid is added and neutralizes, stirs 8 points
Clock is added 180Kg toluene and is extracted, and then stops stirring standing after 15 minutes, is discharged, adds from reactor bottom valve by waste water
Enter oxalic acid 1.0kg, be then turned on stirring and 80Kg tap water is added, stir 10 minutes, then stops stirring standing after 18 minutes, equally
Be discharged from reactor bottom valve by waste water, detect pH ≈ 7-7.5, normal pressure desolventizing, temperature recovery to 160 DEG C, vacuumize-
0.080MPa, softening point reach 95-100 DEG C of blowing and obtain p-tert-butylphenol formaldehyde resin.
Embodiment 5
Stirring is opened, the formalin that 100Kg content is 37% is put into reaction kettle under normal pressure, is then by 10Kg content
25% ammonium hydroxide is added in reaction kettle, and then at a temperature of 50-55 DEG C, 100Kg p-tert-butylphenol is uniformly added into 98 minutes,
It is warming up within 60 minutes later boiling, fluidized state is kept for 180 minutes, is cooled to 60 DEG C, and 4.5Kg acetic acid is added and neutralizes, stirs 5 points
Clock is added 180Kg toluene and is extracted, and then stops stirring standing after 15 minutes, is discharged, adds from reactor bottom valve by waste water
Enter oxalic acid 1.5kg, be then turned on stirring and 70Kg tap water is added, stir 5 minutes, then stops stirring standing after 15 minutes, equally
Be discharged from reactor bottom valve by waste water, detect pH ≈ 7-7.5, normal pressure desolventizing, temperature recovery to 150 DEG C, vacuumize-
0.082MPa, softening point reach 95-100 DEG C of blowing and obtain p-tert-butylphenol formaldehyde resin.
Embodiment 6
Stirring is opened, the formalin that 120Kg content is 37% is put into reaction kettle under normal pressure, is then by 9Kg content
25% ammonium hydroxide is added in reaction kettle, and then at a temperature of 50-55 DEG C, 100Kg p-tert-butylphenol is uniformly added into 90 minutes,
It is warming up within 70 minutes later boiling, fluidized state is kept for 150 minutes, is cooled to 65 DEG C, and 4.0Kg acetic acid is added and neutralizes, stirs 6 points
Clock is added 180Kg toluene and is extracted, and then stops stirring standing after 15 minutes, is discharged, adds from reactor bottom valve by waste water
Enter oxalic acid 2kg, be then turned on stirring be added 80Kg tap water, stir 10 minutes, then stop stirring stand after ten minutes, equally from
Waste water is discharged reactor bottom valve, detect pH ≈ 7-7.5, normal pressure desolventizing, temperature recovery to 145 DEG C, vacuumize-
0.080MPa, softening point reach 95-100 DEG C of blowing and obtain p-tert-butylphenol formaldehyde resin.
Claims (3)
1. a kind of synthesis technology of p tert butylphenol formaldehyde resin, comprising the following steps:
Stirring is opened, under normal pressure puts into formalin in reaction kettle, then ammonium hydroxide is added in reaction kettle；Then in 50-
At a temperature of 55 DEG C, it is uniformly added into p-tert-butylphenol in 90-100 minutes, is warming up to boiling later, fluidized state keeps 150-
180 minutes；It is cooled to 60-65 DEG C, acetic acid is added and neutralizes, stirs 5-10 minutes, toluene is added and is extracted；Then stop to stir quiet
After setting layering in 10-20 minutes, it is discharged from reactor bottom valve by the waste water of lower layer；Oxalic acid is added, is then turned on stirring and is added
Tap water stirs 5-10 minutes；Then stop after stirring stands 10-20 minute and be layered, equally from reactor bottom valve by lower layer
Waste water discharge；PH ≈ 7-7.5 is detected, normal pressure desolventizing toluene, temperature recovery is to 140-160 DEG C；Vacuumize-0.080 ----
0.085MPa, vacuum pumping blowing obtain t-Butylphenol formaldehyde resin.
2. p tert butylphenol formaldehyde resin synthesis technology as described in claim 1, it is characterised in that: the addition is to tertiary fourth
Base phenol, the time for being warming up to boiling later controlled at 60-70 minutes.
3. p tert butylphenol formaldehyde resin synthesis technology as described in claim 1, it is characterised in that: used each component
Weight be divided into:
100 parts by weight of p-tert-butylphenol,
The formalin be 100-120 parts by weight and content be 37%,
The ammonium hydroxide be 8-10 parts by weight and content be 25%,
The acetic acid be 3.5-4.5 parts by weight,
180 parts by weight of toluene,
The industrial ethanedioic acid be 1-2 parts by weight and 99% or more content,
The tap water 70-80 parts by weight.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201910648203.4A CN110330610A (en) | 2019-07-18 | 2019-07-18 | A kind of synthesis technology of p tert butylphenol formaldehyde resin |
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| CN201910648203.4A CN110330610A (en) | 2019-07-18 | 2019-07-18 | A kind of synthesis technology of p tert butylphenol formaldehyde resin |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111116852A (en) * | 2019-12-18 | 2020-05-08 | 杭摩新材料集团股份有限公司 | Solvent-free preparation method of thermal reaction type p-tert-butylphenol resin |
| CN112110420A (en) * | 2020-09-04 | 2020-12-22 | 上海交通大学 | Method for catalytically synthesizing hydrogen peroxide by using visible light to drive aminophenol formaldehyde resin |
| CN112175155A (en) * | 2020-08-17 | 2021-01-05 | 杭摩新材料集团股份有限公司 | Special phenolic resin for nylon cord fabric and production method thereof |
| CN114317973A (en) * | 2021-12-17 | 2022-04-12 | 北京工业大学 | Pyrolysis recovery method for organic components of waste light-emitting diodes |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111116852A (en) * | 2019-12-18 | 2020-05-08 | 杭摩新材料集团股份有限公司 | Solvent-free preparation method of thermal reaction type p-tert-butylphenol resin |
| CN112175155A (en) * | 2020-08-17 | 2021-01-05 | 杭摩新材料集团股份有限公司 | Special phenolic resin for nylon cord fabric and production method thereof |
| CN112175155B (en) * | 2020-08-17 | 2022-10-14 | 杭摩新材料集团股份有限公司 | Special phenolic resin for nylon cord fabric and production method thereof |
| CN112110420A (en) * | 2020-09-04 | 2020-12-22 | 上海交通大学 | Method for catalytically synthesizing hydrogen peroxide by using visible light to drive aminophenol formaldehyde resin |
| CN114317973A (en) * | 2021-12-17 | 2022-04-12 | 北京工业大学 | Pyrolysis recovery method for organic components of waste light-emitting diodes |
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Application publication date: 20191015 |