CN110527041A - A kind of synthetic method of phenolic resin - Google Patents
A kind of synthetic method of phenolic resin Download PDFInfo
- Publication number
- CN110527041A CN110527041A CN201910969881.0A CN201910969881A CN110527041A CN 110527041 A CN110527041 A CN 110527041A CN 201910969881 A CN201910969881 A CN 201910969881A CN 110527041 A CN110527041 A CN 110527041A
- Authority
- CN
- China
- Prior art keywords
- phenol
- phenolic resin
- synthetic method
- reaction
- mixed
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
- C08G8/10—Condensation polymers of aldehydes or ketones with phenols only of aldehydes of formaldehyde, e.g. of formaldehyde formed in situ with phenol
-
- 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
- C08G8/24—Condensation polymers of aldehydes or ketones with phenols only of aldehydes of formaldehyde, e.g. of formaldehyde formed in situ with mixtures of two or more phenols which are not covered by only one of the groups C08G8/10 - C08G8/20
-
- 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
- C08G8/28—Chemically modified polycondensates
- C08G8/32—Chemically modified polycondensates by organic acids or derivatives thereof, e.g. fatty oils
-
- 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
- C08G8/28—Chemically modified polycondensates
- C08G8/34—Chemically modified polycondensates by natural resins or resin acids, e.g. rosin
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Phenolic Resins Or Amino Resins (AREA)
Abstract
The present invention provides a kind of synthetic methods of phenolic resin, first phenol is heated and obtains melting phenol, catalyst is dissolved in formalin again, it is uniformly mixed, mixed liquor is set to flow, mix in the reaction tube of microchannel with phenol, then the four-hole boiling flask with stirring is continuously entered, reacted, heat preservation, dehydration, termination, vacuum distillation obtain phenolic resin；Modifying agent can also be added after dewatering, obtain phenol-formaldehyde resin modified by terminating, being evaporated under reduced pressure later.In synthetic method of the invention, crystalline state under phenol room temperature, heating melting are convenient for charging at liquid first；Further more, catalyst and formalin are configured to mixed material, which is two bursts of chargings, by being pre-mixed raw material and continuous feed using microchannel reaction tube, improves the mass transfer and heat transfer efficiency of reaction process, and then improve the reaction efficiency of entire technical process.Reaction process is foreshortened to 1-2 hours from the 3-5 hour of original technology.
Description
Technical field
The present invention relates to a kind of synthetic methods of phenol-formaldehyde resin modified, in particular belong to a kind of synthesis side of phenolic resin
Method.
Background technique
Natural rubber, the hardness of synthetic rubber (such as butadiene-styrene rubber, nitrile rubber), elasticity modulus are all lower, Wu Faman
The actual application demand of foot, it is therefore desirable to add reinforcing agent in sizing material to improve its hardness and elastic modulus.Reinforcing agent refers to
The auxiliary agent of sizing material hardness, dynamic modulus can be improved, traditionally improving sizing material hardness is to improve the ratio of supporting material (such as carbon black),
But this method can bring a series of technological problems, and reinforced resin is used then to can avoid these problems.
Phenol Resin as Rubber Reinforcing Filler generally comprises unmodified phenolic resin, cashew nut oil modified alkyd resin, tall oil and changes
Property phenolic resin.Wherein, unmodified phenolic resin polarity is big, water absorption rate is high, and good benefit is not achieved in the poor compatibility with rubber
Potent fruit, and the phenolic resin that oil is modified reduces the polarity of phenolic resin, increases interpenetrating networks density, it is easier to be scattered in
Rubber, reinforcing effect are more preferable.It can be used for tire bead position, tyre surface, it can also be used to the products such as conveyer belt, V-belt, sealing strip,
Especially it is widely applied in radial triangle rubber.The production technology of existing phenol-formaldehyde resin modified, there are the reaction time it is long,
The problems such as low efficiency, improves the competitiveness of domestic relevant enterprise and product, is conducive to China so improving to prior art
The development of functional rubber auxiliary agent industry.
Summary of the invention
The present invention provides a kind of synthetic methods of phenolic resin, to reach the mass transfer and heat transfer effect that improve in reaction process
Rate shortens the purpose in reaction time.
A kind of synthetic method of phenolic resin, which comprises the following steps:
Step 1: phenol being heated, the phenol melted at 50-60 DEG C, kept the temperature spare；It is 37% by mass fraction
Formalin uniformly mixed with catalyst, be mixed raw material, stand for standby use；The molar ratio of the phenol and formaldehyde is 1:
0.6~0.8, the catalyst accounts for the 0.1%~1.0% of phenol quality；
Step 2: step 1 gained mixed raw material being flowed and mixed in the reaction tube of microchannel with phenol, water-bath temperature control exists
70~100 DEG C；The reacted pipe end of material continuously enters in four-hole boiling flask, and the material enters the feed time of four-hole boiling flask
For 10~60min, residence time of the material in reaction tube is 5-30s；Charging be stirred simultaneously simultaneously oil bath temperature control 80~
110 DEG C, continues to stir after charging and keep the temperature 10-40min；
Step 3: after heat preservation, reaction unit being changed to distillation state and carries out thermal dehydration, through terminator, vacuum is added
Distillation obtains phenolic resin.
Preferably, the molar ratio of the phenol and formaldehyde is 1:0.7；The catalyst accounts for the 0.3% of phenol quality.
Preferably, the catalyst is strongly acidic catalyst, is one of sulfuric acid, phosphoric acid, p-methyl benzenesulfonic acid.
Preferably, in the melting phenol in the step 1 be added m-cresol solution mixed, keep the temperature later it is spare,
The additional amount of m-cresol solution and the mass ratio of phenol are 5-9:100.
Preferably, the internal diameter of microchannel reaction tube is 0.8mm in the step 2, is stainless steel material；Microchannel plate is answered
The water-bath control temperature of pipe is 80 DEG C；The feed time that material enters four-hole boiling flask is 30min；Stop of the material in reaction tube
Time is 15s；The temperature of four-hole boiling flask is 95 DEG C by oil bath control temperature；Soaking time is 30min.
Preferably, in the step 3, thermal dehydration temperature is 120 DEG C.
Preferably, in the step 3, thermal dehydration temperature is 160 DEG C, changes back stream and modifying agent is added and reacted,
After terminator, vacuum distillation be added obtain phenol-formaldehyde resin modified.
Preferably, the mass ratio of the modifying agent additional amount and phenol is 0.2~0.6:1；Modifying agent is cashew nut oil, appropriate
One of your oil, rosin, fatty acid；Reaction time after modifying agent is added is 1~2h.
Preferably, the mass ratio of the modifying agent and phenol is 0.4:1.
Preferably, terminator is liquid alkaline that mass fraction is 32%, the molar ratio of catalyst and liquid alkaline in the step 3
For 1:0.5.
Compared with prior art, the present invention advantage is:
It is phenol and catalyst to be previously added to reaction kettle, then be added dropwise in the prior art when preparing phenol-formaldehyde resin modified
Formalin, since phenol in reaction process and formaldehyde carry out addition, polycondensation reaction, two-step reaction under conditions of catalyst
There is no specific boundary, so being continuously added with formalin, reaction generates phenolic aldehyde performed polymer, and viscosity is larger, In
Molecule slow diffusion in whipping process reduces the mass transfer and rate of heat transfer of reaction, and material reaction is insufficient, when so as to cause reaction
Between long, low efficiency.The method of the present invention, which first heats phenol, obtains melting phenol, then catalyst is dissolved in formalin, mixes
It closes uniform.In synthetic method of the invention, crystalline state under phenol room temperature, heating melting are convenient for charging at liquid first；Again
Having, catalyst and formalin are configured to mixed material, which is two bursts of chargings, and it is easy to operate, improve reaction process
Mass transfer and heat transfer efficiency, and then improve the reaction efficiency of entire technical process.
Specific embodiment
The invention will be described in further detail With reference to embodiment, unless otherwise instructed, following embodiments
Each raw material used is commercial product.
Embodiment 1-3 is the preparation method of phenolic resin:
Embodiment 1
Step 1: phenol being heated, the phenol melted at 50 DEG C, it is spare to weigh 50.0g heat preservation；It weighs in proportion
0.15g catalyst is dissolved in 30.4g formalin, is completely dissolved, and is uniformly mixed, and is mixed material, stand for standby use；
Step 2: step 1 gained mixed raw material is flowed and mixed in the reaction tube of microchannel with phenol, water-bath temperature control 80
DEG C, being computed adjusting pump discharge makes feed time 60min, and residence time of the material in reaction tube is 15s；Mixed material warp
Reaction pipe end continuously enters in four-hole boiling flask, feeds while being stirred, and oil bath temperature control is 95 DEG C, continues to stir after charging
Mix heat preservation 40min；
Step 3: being changed to distillation state after heat preservation, be warming up to 120 DEG C of progress thermal dehydrations, add 0.05g liquid alkaline
Reaction is terminated, finally obtains 59.4g phenolic resin by vacuum distillation.It is computed, the yield of phenolic resin is 96.7%.
Embodiment 2
Step 1: phenol being heated, the phenol melted at 60 DEG C, it is spare to weigh 50.0g heat preservation；It weighs in proportion
0.05g catalyst is dissolved in 25.9g formalin, is completely dissolved, and is uniformly mixed, and is mixed material, stand for standby use；
Step 2: step 1 gained mixed raw material is flowed and mixed in the reaction tube of microchannel with phenol, water-bath temperature control 100
DEG C, being computed adjusting pump discharge makes feed time 10min, and residence time of the material in reaction tube is 5s；Mixed material warp
Reaction pipe end continuously enters in four-hole boiling flask, feeds while being stirred, and oil bath temperature control is 80 DEG C, continues to stir after charging
Mix heat preservation 10min；
Step 3: being changed to distillation state after heat preservation, be warming up to 120 DEG C of progress thermal dehydrations, add 0.02g liquid alkaline
Reaction is terminated, finally obtains 49.5g phenolic resin by vacuum distillation.It is computed, the yield of phenolic resin is 88.1%.
Embodiment 3
Step 1: phenol being heated, the phenol melted at 55 DEG C, it is spare to weigh 50.0g heat preservation；It weighs in proportion
0.25g catalyst is dissolved in 34.8g formalin, is completely dissolved, and is uniformly mixed, and is mixed material, stand for standby use；
Step 2: step 1 gained mixed raw material is flowed and mixed in the reaction tube of microchannel with phenol, water-bath temperature control 90
DEG C, being computed adjusting pump discharge makes feed time 40min, and residence time of the material in reaction tube is 30s；Mixed material warp
Reaction pipe end continuously enters in four-hole boiling flask, feeds while being stirred, and oil bath temperature control is 105 DEG C, continues after charging
Stirring heat preservation 20min；
Step 3: being changed to distillation state after heat preservation, be warming up to 120 DEG C of progress thermal dehydrations, add 0.08g liquid alkaline
Reaction is terminated, finally obtains 61.4g phenolic resin by vacuum distillation.It is computed, the yield of phenolic resin is 97.1%.
Phenolic resin obtained by embodiment 1-3 is tested, following project data is obtained:
| Embodiment 1 | Embodiment 2 | Embodiment 3 | |
| Softening point/DEG C | 100.5 | 89.9 | 108.5 |
| Heating loss % | 0.4 | 0.6 | 0.2 |
| Ash content % | 0.06 | 0.01 | 0.09 |
| Yield % | 96.7 | 91.1 | 97.1 |
Embodiment 4-6 is the preparation method for the phenol-formaldehyde resin modified that raw material is phenol:
Embodiment 4
Step 1: phenol being heated, the phenol melted at 50 DEG C, it is spare to weigh 50.0g heat preservation；It weighs in proportion
0.15g catalyst is dissolved in 30.4g formalin, is completely dissolved, and is uniformly mixed, and is mixed material, stand for standby use；
Step 2: step 1 gained mixed raw material is flowed and mixed in the reaction tube of microchannel with phenol, water-bath temperature control 80
DEG C, being computed adjusting pump discharge makes feed time 30min, and residence time of the material in reaction tube is 10s；Mixed material warp
Reaction pipe end continuously enters in four-hole boiling flask, feeds while being stirred, and oil bath temperature control is 105 DEG C, continues after charging
Stirring heat preservation 10min；
Step 3: after heat preservation, reaction unit is changed to distillation state and carries out thermal dehydration, until temperature is up to 160 DEG C,
It changes back stream and is added 20g tall oil the reaction was continued 1.5h, add 0.05g liquid alkaline and terminate reaction, be finally by vacuum distillation
Obtain 79.6g phenol-formaldehyde resin modified.It is computed, the yield of phenol-formaldehyde resin modified is 97.8%.
Embodiment 5
Step 1: phenol being heated, the phenol melted at 60 DEG C, it is spare to weigh 50.0g heat preservation；It weighs in proportion
0.05g catalyst is dissolved in 25.9g formalin, is completely dissolved, and is uniformly mixed, and is mixed material, stand for standby use；
Step 2: step 1 gained mixed raw material is flowed and mixed in the reaction tube of microchannel with phenol, water-bath temperature control 100
DEG C, being computed adjusting pump discharge makes feed time 60min, changes tube length of reaction tube or adjusts flow, makes material in reaction tube
In residence time be 25s；The reacted pipe end of mixed material continuously enters in four-hole boiling flask, feeds while being stirred, oil
Bathing temperature control is 110 DEG C, continues stirring heat preservation 40min after charging；
Step 3: after heat preservation, reaction unit is changed to distillation state and carries out thermal dehydration, until temperature is up to 160 DEG C,
It changes back stream and is added 10g rosin the reaction was continued 1h, add 0.02g liquid alkaline and terminate reaction, finally being obtained by vacuum distillation
63.1g phenol-formaldehyde resin modified.It is computed, the yield of phenol-formaldehyde resin modified is 90.7%.
Embodiment 6
Step 1: phenol being heated, the phenol melted at 55 DEG C, it is spare to weigh 50.0g heat preservation；It weighs in proportion
0.25g catalyst is dissolved in 34.8g formalin, is completely dissolved, and is uniformly mixed, and is mixed material, stand for standby use；
Step 2: step 1 gained mixed raw material is flowed and mixed in the reaction tube of microchannel with phenol, water-bath temperature control 90
DEG C, being computed adjusting pump discharge makes feed time 10min, and residence time of the material in reaction tube is 5s；Mixed material warp
Reaction pipe end continuously enters in four-hole boiling flask, feeds while being stirred, and oil bath temperature control is 80 DEG C, continues to stir after charging
Mix heat preservation 20min；
Step 3: after heat preservation, reaction unit is changed to distillation state and carries out thermal dehydration, until temperature is up to 160 DEG C,
It changes back stream and is added 25g cashew nut oil the reaction was continued 2h, add 0.08g liquid alkaline and terminate reaction, finally by being evaporated in vacuo to obtain the final product
To 85.3g phenol-formaldehyde resin modified.It is computed, the yield of phenol-formaldehyde resin modified is 96.8%.
Phenol-formaldehyde resin modified obtained by embodiment 4-6 is tested, following project data is obtained:
| Embodiment 4 | Embodiment 5 | Embodiment 6 | |
| Softening point/DEG C | 98.5 | 91.7 | 106.3 |
| Heating loss % | 0.5 | 0.55 | 0.35 |
| Ash content % | 0.05 | 0.02 | 0.07 |
| Yield % | 97.8 | 90.7 | 96.8 |
Embodiment 7-9 is the preparation method for the phenol-formaldehyde resin modified that raw material is in phenol added with metacresol:
Embodiment 7
Step 1: phenol being heated at 50 DEG C, weighs the phenol of 50.0g melting, 4g metacresol is added, is kept the temperature spare；It presses
Ratio weighs 0.15g catalyst and is dissolved in 30.4g formalin, is completely dissolved, and uniformly mixes, and is mixed material, stands standby
With；
Step 2: two bursts of mixed raw materials described in step 1 are flowed and mixed in the reaction tube of microchannel, 70 DEG C of water-bath temperature control,
Being computed adjusting pump discharge makes feed time 30min, and residence time of the material in reaction tube is 15s；Mixed material is through anti-
It answers pipe end to continuously enter in four-hole boiling flask, feed while being stirred, oil bath temperature control is 95 DEG C, continues to stir after charging
Keep the temperature 30min；
Step 3: after heat preservation, reaction unit is changed to distillation state and carries out thermal dehydration, until temperature is up to 160 DEG C,
It changes back stream and is added 20g tall oil the reaction was continued 2h, add 0.05g liquid alkaline and terminate reaction, finally by being evaporated in vacuo to obtain the final product
To 83.3g phenol-formaldehyde resin modified.It is computed, the yield of phenol-formaldehyde resin modified is 97.5%.
Embodiment 8
Step 1: phenol being heated at 50 DEG C, weighs the phenol of 50.0g melting, 2.5g metacresol is added；Claim in proportion
It takes 0.05g catalyst to be dissolved in 25.9g formalin, is completely dissolved, uniformly mix, be mixed material, stand for standby use；
Step 2: two bursts of mixed raw materials obtained by step 1 are flowed and mixed in the reaction tube of microchannel, 80 DEG C of water-bath temperature control,
Being computed adjusting pump discharge makes feed time 10min, and residence time of the material in reaction tube is 5s；Mixed material is reacted
Pipe end continuously enters in four-hole boiling flask, feeds while being stirred, and oil bath temperature control is 80 DEG C, continues stirring after charging and protects
Warm 10min；
Step 3: after heat preservation, reaction unit is changed to distillation state and carries out thermal dehydration, until temperature is up to 160 DEG C,
It changes back stream and is added 10g cashew nut oil the reaction was continued 1h, add 0.02g liquid alkaline and terminate reaction, finally by being evaporated in vacuo to obtain the final product
To 65.9g phenol-formaldehyde resin modified.It is computed, the yield of phenol-formaldehyde resin modified is 91.4%.
Embodiment 9
Step 1: phenol being heated at 50 DEG C, weighs the phenol of 50.0g melting, 4.5g metacresol is added, is kept the temperature spare；
0.25g catalyst is weighed in proportion to be dissolved in 34.8g formalin, is completely dissolved, is uniformly mixed, and is mixed material, is stood
It is spare；
Step 2: two bursts of mixed raw materials obtained by step 1 are flowed and mixed in the reaction tube of microchannel, 90 DEG C of water-bath temperature control,
Being computed adjusting pump discharge makes feed time 40min, and residence time of the material in reaction tube is 15s；Mixed material is through anti-
It answers pipe end to continuously enter in four-hole boiling flask, feed while being stirred, oil bath temperature control is 105 DEG C, continues to stir after charging
Mix heat preservation 20min；
Step 3: after heat preservation, reaction unit is changed to distillation state and carries out thermal dehydration, until temperature is up to 160 DEG C,
It changes back stream and is added 25g fatty acid the reaction was continued 1.5h, add 0.08g liquid alkaline and terminate reaction, be finally by vacuum distillation
Obtain 87.3g phenol-formaldehyde resin modified.It is computed, the yield of phenol-formaldehyde resin modified is 94.2%.
Phenol-formaldehyde resin modified obtained by embodiment 7-9 is tested, following project data is obtained:
1-9 is obtained in conjunction with the embodiments phenolic resin and phenol-formaldehyde resin modified it is found that by building microchannel reaction tube with
The tandem arrangement of four-hole boiling flask, realization are pre-mixed material and continuous feed, improve the mass-and heat-transfer efficiency of reaction process, by the
Single step reaction and soaking time foreshorten to 1-2 hours from the 3-5 hour of original technology, and can obtain in high yield, are phenolic resin
Synthesis provide a kind of new synthetic method.
Claims (10)
1. a kind of synthetic method of phenolic resin, which comprises the following steps:
Step 1: phenol being heated, the phenol melted at 50-60 DEG C, kept the temperature spare；The first for being 37% by mass fraction
Aldehyde aqueous solution is uniformly mixed with catalyst, is mixed raw material, stand for standby use；The molar ratio of the phenol and formaldehyde is 1:0.6
~0.8, the catalyst accounts for the 0.1%~1.0% of phenol quality；
Step 2: step 1 gained mixed raw material is flowed and is mixed in the reaction tube of microchannel with phenol, water-bath temperature control 70~
100℃；The reacted pipe end of material continuously enters in four-hole boiling flask, and the feed time that the material enters four-hole boiling flask is 10
~60min, residence time of the material in reaction tube are 5-30s；Charging simultaneously be stirred simultaneously oil bath temperature control 80~110
DEG C, continue to stir after charging and keeps the temperature 10-40min；
Step 3: after heat preservation, reaction unit being changed to distillation state and carries out thermal dehydration, terminator, vacuum distillation is added
Obtain phenolic resin.
2. the synthetic method of phenolic resin according to claim 1, which is characterized in that mole of the phenol and formaldehyde
Than for 1:0.7；The catalyst accounts for the 0.3% of phenol quality.
3. the synthetic method of phenolic resin according to claim 1, which is characterized in that the catalyst is urged for highly acid
Agent is one of sulfuric acid, phosphoric acid, p-methyl benzenesulfonic acid.
4. the synthetic method of phenolic resin according to claim 1, which is characterized in that the melting benzene in the step 1
M-cresol solution is added in phenol to be mixed, keeps the temperature later spare, the mass ratio of the additional amount of m-cresol solution and phenol is 5-
9:100。
5. the synthetic method of phenolic resin according to claim 1, which is characterized in that microchannel plate in the step 2
Should pipe internal diameter be 0.8mm, be stainless steel material；The water-bath control temperature of microchannel reaction tube is 80 DEG C；Material enters four mouthfuls
The feed time of flask is 30min；Residence time of the material in reaction tube is 15s；The temperature of four-hole boiling flask passes through oil bath control
Temperature is 95 DEG C；Soaking time is 30min.
6. the synthetic method of phenolic resin according to claim 1, which is characterized in that in the step 3, thermal dehydration
Temperature is 120 DEG C.
7. the synthetic method of phenolic resin according to claim 1, which is characterized in that in the step 3, thermal dehydration
Temperature is 160 DEG C, changes back stream and modifying agent is added and reacted, after terminator is added, vacuum distillation obtains modified phenol
Urea formaldehyde.
8. the synthetic method of phenolic resin according to claim 7, which is characterized in that the modifying agent additional amount and benzene
The mass ratio of phenol is 0.2~0.6:1；Modifying agent is one of cashew nut oil, tall oil, rosin, fatty acid；After modifying agent is added
Reaction time be 1~2h.
9. the synthetic method of phenolic resin according to claim 8, which is characterized in that the matter of the modifying agent and phenol
Amount is than being 0.4:1.
10. the synthetic method of phenolic resin according to claim 1, which is characterized in that terminator is in the step 3
The molar ratio of the liquid alkaline that mass fraction is 32%, catalyst and liquid alkaline is 1:0.5.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910969881.0A CN110527041A (en) | 2019-10-12 | 2019-10-12 | A kind of synthetic method of phenolic resin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910969881.0A CN110527041A (en) | 2019-10-12 | 2019-10-12 | A kind of synthetic method of phenolic resin |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110527041A true CN110527041A (en) | 2019-12-03 |
Family
ID=68671714
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910969881.0A Pending CN110527041A (en) | 2019-10-12 | 2019-10-12 | A kind of synthetic method of phenolic resin |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110527041A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112552472A (en) * | 2020-11-13 | 2021-03-26 | 山东京博木基材料有限公司 | Preparation method of water-soluble toughened modified phenolic resin |
| CN114685742A (en) * | 2020-12-31 | 2022-07-01 | 上海昶法新材料有限公司 | Preparation method of phenolic resin |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101230121A (en) * | 2007-12-20 | 2008-07-30 | 武汉径河化工有限公司 | Preparation method of tall oil modified alkyd resin |
| CN102558473A (en) * | 2011-12-28 | 2012-07-11 | 北京彤程创展科技有限公司 | Cashew nut oil-modified phenolic resin and preparation method thereof |
| CN102993390A (en) * | 2012-10-08 | 2013-03-27 | 山东莱芜润达新材料有限公司 | Continuous production method of thermoplastic phenolic resin |
| CN103910842A (en) * | 2013-01-09 | 2014-07-09 | 华奇（张家港）化工有限公司 | Tall oil modified phenolic resin and preparation method and application thereof |
| CN103910841A (en) * | 2013-01-09 | 2014-07-09 | 华奇（张家港）化工有限公司 | Tall oil modified phenolic resin and preparation method thereof |
| CN104327227A (en) * | 2014-11-18 | 2015-02-04 | 西安元创化工科技股份有限公司 | Method for synthesizing phenolic resin |
| CN106554475A (en) * | 2016-11-30 | 2017-04-05 | 黄河三角洲京博化工研究院有限公司 | A kind of phenolic resin synthesizer and phenolic resin synthetic method |
| WO2019156154A1 (en) * | 2018-02-08 | 2019-08-15 | 日本化薬株式会社 | Photosensitive resin composition and cured product of same |
-
2019
- 2019-10-12 CN CN201910969881.0A patent/CN110527041A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101230121A (en) * | 2007-12-20 | 2008-07-30 | 武汉径河化工有限公司 | Preparation method of tall oil modified alkyd resin |
| CN102558473A (en) * | 2011-12-28 | 2012-07-11 | 北京彤程创展科技有限公司 | Cashew nut oil-modified phenolic resin and preparation method thereof |
| CN102993390A (en) * | 2012-10-08 | 2013-03-27 | 山东莱芜润达新材料有限公司 | Continuous production method of thermoplastic phenolic resin |
| CN103910842A (en) * | 2013-01-09 | 2014-07-09 | 华奇（张家港）化工有限公司 | Tall oil modified phenolic resin and preparation method and application thereof |
| CN103910841A (en) * | 2013-01-09 | 2014-07-09 | 华奇（张家港）化工有限公司 | Tall oil modified phenolic resin and preparation method thereof |
| CN104327227A (en) * | 2014-11-18 | 2015-02-04 | 西安元创化工科技股份有限公司 | Method for synthesizing phenolic resin |
| CN106554475A (en) * | 2016-11-30 | 2017-04-05 | 黄河三角洲京博化工研究院有限公司 | A kind of phenolic resin synthesizer and phenolic resin synthetic method |
| WO2019156154A1 (en) * | 2018-02-08 | 2019-08-15 | 日本化薬株式会社 | Photosensitive resin composition and cured product of same |
Non-Patent Citations (1)
| Title |
|---|
| 橡胶工业原材料与装备简明手册编审委员会编著: "《橡胶工业原材料与装备简明手册 原材料与工艺耗材分册》", 31 January 2019, 北京理工大学出版社 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112552472A (en) * | 2020-11-13 | 2021-03-26 | 山东京博木基材料有限公司 | Preparation method of water-soluble toughened modified phenolic resin |
| CN112552472B (en) * | 2020-11-13 | 2022-08-16 | 山东京博木基材料有限公司 | Preparation method of water-soluble toughened modified phenolic resin |
| CN114685742A (en) * | 2020-12-31 | 2022-07-01 | 上海昶法新材料有限公司 | Preparation method of phenolic resin |
| CN114685742B (en) * | 2020-12-31 | 2024-03-29 | 上海昶法新材料有限公司 | Preparation method of phenolic resin |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110527041A (en) | A kind of synthetic method of phenolic resin | |
| CN102121208B (en) | Method for preparing papermaking dry strengthening agent | |
| CN102250363B (en) | Modification method of lignin | |
| CN101368074A (en) | Starch adhesive agent and preparation method thereof | |
| CN103087280B (en) | Method for synthesizing phenolic resins by using paraformaldehyde | |
| CN105504267A (en) | Three-phase hydrolytic polymerization process for nylon 6 | |
| CN106750062A (en) | A kind of phenolic resin of modified by cardanol and the preparation method of phenolaldehyde moulding compound | |
| CN105237667A (en) | Preparation method of styrene-butadiene latex for carpets | |
| CN107128914A (en) | The preparation method of petroleum coke pilum shaped activated carbon | |
| CN104788633B (en) | A kind of phenolic resin modified Lauxite and preparation method thereof | |
| CN102199265B (en) | Long carbon chain nylon modified phenolic resin and preparation method thereof | |
| CN105566590B (en) | A kind of preparation method and applications of phenol-formaldehyde resin modified | |
| CN107200994A (en) | A kind of preparation method of the composite modified phenol formaldehyde resin of anacardol and nitrile rubber | |
| CN106380887A (en) | Preparation method of lignin-base phenolic aldehyde molding compound | |
| CN111205799B (en) | Production process of cardanol modified phenolic resin adhesive | |
| CN104629551A (en) | Production method for producing high-impact-resistance polyvinyl chloride resin anti-sticking kettle agent | |
| CN105085849B (en) | A kind of modified resorcinol formaldehyde resin adhesion promotor and preparation method thereof | |
| CN106750070B (en) | A kind of type thermosetting resin wetting agent and its preparation method and application | |
| CN112321779B (en) | Continuous production method of water-soluble phenolic resin | |
| CN102108115A (en) | Phenolic resin for environment-friendly thermoplastic refractory material and preparation method thereof | |
| CN114805715A (en) | Novel phenolic resin and application thereof in preparation of flexible graphite-based bipolar plate | |
| CN106750066A (en) | A kind of preparation method of the phenolic resin of modified by cardanol | |
| CN106496471B (en) | The preparation method of the high ortho position thermosetting property pultrusion phenolic resin of one pack system | |
| CN208727480U (en) | A kind of reactor tank with agitating device | |
| CN111333796A (en) | Preparation method of tetraphenol ethane phenolic resin |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20191203 |