CN108676321A - The method that polyvinyl butyral is modified magnesium phenolic aldehyde is prepared based on solid formaldehyde - Google Patents
The method that polyvinyl butyral is modified magnesium phenolic aldehyde is prepared based on solid formaldehyde Download PDFInfo
- Publication number
- CN108676321A CN108676321A CN201810532091.1A CN201810532091A CN108676321A CN 108676321 A CN108676321 A CN 108676321A CN 201810532091 A CN201810532091 A CN 201810532091A CN 108676321 A CN108676321 A CN 108676321A
- Authority
- CN
- China
- Prior art keywords
- phenolic aldehyde
- pvb
- solid formaldehyde
- phenol
- magnesium phenolic
- 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.)
- Withdrawn
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L61/00—Compositions of condensation polymers of aldehydes or ketones; Compositions of derivatives of such polymers
- C08L61/04—Condensation polymers of aldehydes or ketones with phenols only
- C08L61/06—Condensation polymers of aldehydes or ketones with phenols only of aldehydes with phenols
- C08L61/14—Modified phenol-aldehyde condensates
-
- 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
- C08G8/28—Chemically modified polycondensates
Abstract
The method that polyvinyl butyral is modified magnesium phenolic aldehyde is prepared based on solid formaldehyde the invention discloses a kind of, is related to novolak resin technical field.The present invention includes preparing the modification magnesium phenolic aldehyde to be made of phenol, solid formaldehyde, magnesia, catalyst, PVB, inner pattern releasing agent applicable；Prepare the following process of method of the modification magnesium phenolic aldehyde：PVB is dissolved into 10% 15% alcoholic solution it is spare；The phenol melted and magnesia stirring is added；When 60 DEG C of temperature of charge or less, solid formaldehyde and catalyst is added and stirs；When material react at 80 100 DEG C 2 it is small when after, gel time is surveyed in sampling；After gel time qualification, PVB solution and inner pattern releasing agent applicable stirring is added, is cooled to 60 DEG C or less blowings.The method that the present invention prepares modified magnesium phenolic resin has many advantages, such as to improve production efficiency, reduced cost, with no exhaust gas, zero waste water, reduction energy consumption.
Description
Technical field
The invention belongs to novolak resin technical fields, and polyvinyl alcohol is prepared based on solid formaldehyde more particularly to one kind
The method that butyral is modified magnesium phenolic resin, reacts under the action of basic catalyst especially by phenols and aldehydes and is generated
A kind of thermosetting phenolic high molecular polymer.
Background technology
PVB (polyvinyl butyral, polyvinyl butyral) is not also in fact at present special in China application
Extensively, wherein being mainly plasticized a kind of high molecular material --- the PVB intermediate coats of extrusion forming through plasticizer.PVB is modified magnesium PF's
PF moulding compounds, due to excellent performances such as intensity height, good electrical insulating property, high temperature resistant, acid and alkali-resistances, always in military project and the common people
There is good application with field.
Previous production technology is：
1. phenol and magnesia mixing；
2. liquid formaldehyde and catalyst is added；
3. material reaction 30 minutes viscosimetrics (repeated multiple times until viscosity is up to standard) to after boiling；
4. (time is very long, and generally at 2-3 hours, dehydration, which is not thorough, can influence product finished product for decompression dehydration after viscosity is up to standard
Rate and dimensional stability)；
5. the sticky situation depending on material surveys gel time at any time, after to be drained off and gel time all reaches corresponding reasonable value
PVB solution and inner pattern releasing agent applicable mixing is added in (sometimes water abjection is seldom, and gel time is but very short, the bad control of this process)；
6. waiting for that temperature of charge drops to 60 DEG C of blowings below；
Above method has some drawbacks：1. boiling reaction can make formaldehyde gas escape pollution air；2. having in liquid formaldehyde
Large quantity of moisture, decompression abjection moisture contain aldehyde containing phenol in the middle, and processing is difficult；3. dewatering time is long (2-3 hours general), energy charge
When, low production efficiency influences the quality of product.
Under the energy-efficient overall situation of current national attaching importance to environmental protection, production technology is improved, energy-saving and emission-reduction are enterprise development existence
Deciding factor.The present invention is phenol and solid formaldehyde low-temp reaction, and no dehydration realizes zero emission substantially,
It is with short production cycle, improve production efficiency, it will active influence is generated to PF manufacturing enterprises.
Invention content
The purpose of the present invention is to provide the method that polyvinyl butyral is modified magnesium phenolic aldehyde is prepared based on solid formaldehyde, lead to
It crosses and the method that polyvinyl butyral is modified magnesium phenolic resin is prepared based on solid formaldehyde, especially by phenols and aldehydes in alkalinity
A kind of phenolic aldehyde high molecular polymer for reacting and generating under the action of catalyst solves existing modified magnesium phenolic aldehyde preparation process
Middle dewatering time length, high energy consumption, generates the problems such as pollution at low production efficiency.
In order to solve the above technical problems, the present invention is achieved by the following technical solutions：
The present invention is a kind of method preparing polyvinyl butyral modification magnesium phenolic aldehyde based on solid formaldehyde,
The modification magnesium phenolic aldehyde is prepared to be made of phenol, solid formaldehyde, magnesia, catalyst, PVB, inner pattern releasing agent applicable；
The phenol, formaldehyde, magnesia, catalyst, PVB, inner pattern releasing agent applicable weight ratio be：100：(35-50)：(5-
10)：(3-5)：(15-25)：(3-5)；
Wherein, catalyst is ammonium hydroxide or aniline or the two mixture；Inner pattern releasing agent applicable is animals and plants oleic acid or vegetable and animals oils.
The method for preparing the modification magnesium phenolic aldehyde comprises the following processes：
The alcoholic solution that PVB is dissolved into 10%-15% by SS01 is spare；
SS02 controls reaction kettle medium temperature, and the phenol melted is added and magnesia stirs 20-50 minutes；
When 60 DEG C of temperature of charge or less solid formaldehyde and catalyst is added, and stir in SS03；
SS04 controls temperature of charge to react 2-3 hours at 80 DEG C -100 DEG C, and after material is when reaction 2 is small, sampling is surveyed
Gel time；
SS05 is added PVB solution and inner pattern releasing agent applicable stirring, is cooled to 60 DEG C or less after gel time qualification；
SS06 blowings.
Further, medium is water or oil, range of the control temperature at 60 DEG C -80 DEG C in the step SS02.
Further, range of the phenol control temperature melted in the step SS02 at 60 DEG C -80 DEG C.
The invention has the advantages that：
1. there is the method that the present invention prepares modified magnesium phenolic resin low-temp reaction, formaldehydeless gas to escape, not pollute sky
Gas.
2. the present invention prepare the method for modified magnesium phenolic resin with no dehydration, without waste water generation, wastewater zero discharge,
Protect environment.
It saves dewatering time 3. the method that the present invention prepares modified magnesium phenolic resin has, production time shortening, improve
Production efficiency.
4. the method that the present invention prepares modified magnesium phenolic resin improves production efficiency, reduced cost, with no exhaust gas, zero
Waste water, the advantages that reducing energy consumption and improving production efficiency.
Certainly, it implements any of the products of the present invention and does not necessarily require achieving all the advantages described above at the same time.
Description of the drawings
In order to illustrate the technical solution of the embodiments of the present invention more clearly, will be described below to embodiment required
Attached drawing is briefly described, it should be apparent that, drawings in the following description are only some embodiments of the invention, for ability
For the those of ordinary skill of domain, without creative efforts, it can also be obtained according to these attached drawings other attached
Figure.
Fig. 1 is the flow chart for preparing modified magnesium phenolic resin.
Specific implementation mode
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation describes, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, those of ordinary skill in the art are obtained all other without creative efforts
Embodiment shall fall within the protection scope of the present invention.
Thermoplastic resin：Polyvinyl butyral, english abbreviation PVB resin, molecular formula：C14H18 Cl N3 S
Embodiment one
The present invention is a kind of method preparing polyvinyl butyral modification magnesium phenolic aldehyde based on solid formaldehyde,
The modification magnesium phenolic aldehyde is prepared to be made of phenol, solid formaldehyde, magnesia, catalyst, PVB, inner pattern releasing agent applicable；
Wherein, the weight ratio that phenol, formaldehyde, magnesia, catalyst, PVB, inner pattern releasing agent applicable use for：100：35：5：3：
15：3；Catalyst is ammonium hydroxide；Inner pattern releasing agent applicable is animals and plants oleic acid.
Refering to Figure 1, the method for preparing the modification magnesium phenolic aldehyde comprises the following processes：
The alcoholic solution that PVB is dissolved into 10% by SS01 is spare；
SS02 controls reaction kettle medium temperature, and medium is water or oil, control temperature at 60 DEG C, be added the phenol that has melted and
Magnesia stirs 20 minutes, range of the phenol control temperature melted at 60 DEG C；
When 60 DEG C of temperature of charge or less solid formaldehyde and catalyst is added, and stir in SS03；
The control of SS04 temperature of charge is reacted 2-3 hours at 80 DEG C, and after material is when reaction 2 is small, gel time is surveyed in sampling；
There is the reaction process low-temp reaction, formaldehydeless gas to escape, not pollute air；
SS05 is added PVB solution and inner pattern releasing agent applicable stirring, is cooled to 60 DEG C or less after gel time qualification；
SS06 blowings.
The above process, at low ambient temperatures, reaction time are longer, and gel time is at 85-100s/165 DEG C, formed product
Slowly, efficiency is low, and solid content is 50%~60%.
Embodiment two
The present invention is a kind of method preparing polyvinyl butyral modification magnesium phenolic aldehyde based on solid formaldehyde,
The modification magnesium phenolic aldehyde is prepared to be made of phenol, solid formaldehyde, magnesia, catalyst, PVB, inner pattern releasing agent applicable；
Phenol, formaldehyde, magnesia, catalyst, PVB, inner pattern releasing agent applicable weight ratio be：100：42：7.5:4：20：4；Catalysis
Agent is aniline or the two mixture；Inner pattern releasing agent applicable is vegetable and animals oils.
Refering to Figure 1, the method for preparing the modification magnesium phenolic aldehyde comprises the following processes：
The alcoholic solution that PVB is dissolved into 12.5% by SS01 is spare；
SS02 controls reaction kettle medium temperature, and medium is water or oil, controls range of the temperature at 70 DEG C, what addition had been melted
Phenol and magnesia stir 40 minutes, range of the phenol control temperature melted at 70 DEG C；
When 60 DEG C of temperature of charge or less solid formaldehyde and catalyst is added, and stir in SS03；Wait for gel time qualification
Afterwards, PVB solution and inner pattern releasing agent applicable stirring is added, is cooled to 60 DEG C or less；
The control of SS04 temperature of charge is reacted 2-3 hours at 90 DEG C, and after material is when reaction 2 is small, gel time is surveyed in sampling；
SS05 is added PVB solution and inner pattern releasing agent applicable stirring, is cooled to 60 DEG C or less after gel time qualification；
SS06 blowings.
The above process, under 90 DEG C of warm environment, the reaction time is appropriate, and gel time is at 60-90s/165 DEG C, convenient for controlling,
Solid content is 55%~65%.
Embodiment three
The present invention is a kind of method preparing polyvinyl butyral modification magnesium phenolic aldehyde based on solid formaldehyde,
The modification magnesium phenolic aldehyde is prepared to be made of phenol, solid formaldehyde, magnesia, catalyst, PVB, inner pattern releasing agent applicable；
Phenol, formaldehyde, magnesia, catalyst, PVB, inner pattern releasing agent applicable weight ratio be：100：50：10:5：25：5；Catalysis
Agent is ammonium hydroxide or aniline or the two mixture；Inner pattern releasing agent applicable is animals and plants oleic acid.
Refering to Figure 1, the method for preparing the modification magnesium phenolic aldehyde comprises the following processes：
The alcoholic solution that PVB is dissolved into 15% by SS01 is spare；
SS02 controls reaction kettle medium temperature, and medium is water or oil, controls range of the temperature at 80 DEG C, what addition had been melted
Phenol and magnesia stir 50 minutes, range of the phenol control temperature melted at 60 DEG C -80 DEG C；
When 60 DEG C of temperature of charge or less solid formaldehyde and catalyst is added, and stir in SS03；
SS04 controls temperature of charge to react 2-3 hours at 100 DEG C, after material is when reaction 2 is small, when gel is surveyed in sampling
Between；
SS05 is added PVB solution and inner pattern releasing agent applicable stirring, is cooled to 60 DEG C or less after gel time qualification；
SS06 blowings.
The above process, under high temperature environment, reaction time are short, and gel time is difficult to control, solid at 40-60s/165 DEG C
Content is 60%~70%.
In the description of this specification, the description of reference term " one embodiment ", " example ", " specific example " etc. means
Particular features, structures, materials, or characteristics described in conjunction with this embodiment or example are contained at least one implementation of the present invention
In example or example.In the present specification, schematic expression of the above terms may not refer to the same embodiment or example.
Moreover, particular features, structures, materials, or characteristics described can be in any one or more of the embodiments or examples to close
Suitable mode combines.
Present invention disclosed above preferred embodiment is only intended to help to illustrate the present invention.There is no detailed for preferred embodiment
All details are described, are not limited the invention to the specific embodiments described.Obviously, according to the content of this specification,
It can make many modifications and variations.These embodiments are chosen and specifically described to this specification, is in order to preferably explain the present invention
Principle and practical application, to enable skilled artisan to be best understood by and utilize the present invention.The present invention is only
It is limited by claims and its full scope and equivalent.
Claims (3)
1. preparing the method that polyvinyl butyral is modified magnesium phenolic aldehyde based on solid formaldehyde, it is characterised in that：
The modification magnesium phenolic aldehyde is prepared to be made of phenol, solid formaldehyde, magnesia, catalyst, PVB, inner pattern releasing agent applicable；
The phenol, formaldehyde, magnesia, catalyst, PVB, inner pattern releasing agent applicable weight ratio be：100：(35-50)：(5-10)：(3-
5)：(15-25)：(3-5)；
The method for preparing the modification magnesium phenolic aldehyde comprises the following processes：
The alcoholic solution that PVB is dissolved into 10%-15% by SS01 is spare；
SS02 controls reaction kettle medium temperature, and the phenol melted is added and magnesia stirs 20-50 minutes；
When 60 DEG C of temperature of charge or less solid formaldehyde and catalyst is added, and stir in SS03；
SS04 temperature of charge control 80 DEG C -100 DEG C react 2-3 hour, when material reaction 2 is small after, sampling survey gel time；
SS05 is added PVB solution and inner pattern releasing agent applicable stirring, is cooled to 60 DEG C or less after gel time qualification；
SS06 blowings.
2. according to claim 1 prepare the method that polyvinyl butyral is modified magnesium phenolic aldehyde, spy based on solid formaldehyde
Sign is that medium is water or oil, range of the control temperature at 60 DEG C -80 DEG C in the step SS02.
3. according to claim 1 prepare the method that polyvinyl butyral is modified magnesium phenolic aldehyde, spy based on solid formaldehyde
Sign is that the phenol melted in the step SS02 controls range of the temperature at 60 DEG C -80 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810532091.1A CN108676321A (en) | 2018-05-29 | 2018-05-29 | The method that polyvinyl butyral is modified magnesium phenolic aldehyde is prepared based on solid formaldehyde |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810532091.1A CN108676321A (en) | 2018-05-29 | 2018-05-29 | The method that polyvinyl butyral is modified magnesium phenolic aldehyde is prepared based on solid formaldehyde |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108676321A true CN108676321A (en) | 2018-10-19 |
Family
ID=63807192
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810532091.1A Withdrawn CN108676321A (en) | 2018-05-29 | 2018-05-29 | The method that polyvinyl butyral is modified magnesium phenolic aldehyde is prepared based on solid formaldehyde |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108676321A (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104164050A (en) * | 2014-07-11 | 2014-11-26 | 蚌埠市天宇高温树脂材料有限公司 | Heatproof environmental protection phenolic resin and preparation method of its composite material |
| CN104164051A (en) * | 2014-07-11 | 2014-11-26 | 蚌埠市天宇高温树脂材料有限公司 | Toughening-type environmental protection phenolic resin and preparation method of its composite material |
| CN104194257A (en) * | 2014-07-11 | 2014-12-10 | 蚌埠市天宇高温树脂材料有限公司 | Glass-fiber reinforced molded plastic of heat-resistant environment-friendly phenolic resin |
| CN104194256A (en) * | 2014-07-11 | 2014-12-10 | 蚌埠市天宇高温树脂材料有限公司 | Glass fiber reinforced prepreg prepared from toughened environment-friendly phenolic resin |
| CN106832162A (en) * | 2017-03-13 | 2017-06-13 | 河北泽田化工有限公司 | A kind of silicon and polyethylene glycol double-modification phenolic resin |
-
2018
- 2018-05-29 CN CN201810532091.1A patent/CN108676321A/en not_active Withdrawn
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104164050A (en) * | 2014-07-11 | 2014-11-26 | 蚌埠市天宇高温树脂材料有限公司 | Heatproof environmental protection phenolic resin and preparation method of its composite material |
| CN104164051A (en) * | 2014-07-11 | 2014-11-26 | 蚌埠市天宇高温树脂材料有限公司 | Toughening-type environmental protection phenolic resin and preparation method of its composite material |
| CN104194257A (en) * | 2014-07-11 | 2014-12-10 | 蚌埠市天宇高温树脂材料有限公司 | Glass-fiber reinforced molded plastic of heat-resistant environment-friendly phenolic resin |
| CN104194256A (en) * | 2014-07-11 | 2014-12-10 | 蚌埠市天宇高温树脂材料有限公司 | Glass fiber reinforced prepreg prepared from toughened environment-friendly phenolic resin |
| CN106832162A (en) * | 2017-03-13 | 2017-06-13 | 河北泽田化工有限公司 | A kind of silicon and polyethylene glycol double-modification phenolic resin |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN1300289C (en) | Vegetable oil with high epoxy value and its preparing method and use | |
| CN103319314B (en) | The synthetic method of Bisphenol F under salt bath system | |
| CN102558507B (en) | Raw material of biomass epoxy resin and preparation method of biomass epoxy resin | |
| CN103613728B (en) | Preparation method of lignin phenolic foams | |
| CN103641696B (en) | Method for synthesizing dihydroxypropyl bisphenol A ether through one-step process | |
| CN104387543A (en) | Method for preparing lignin-modified furan resin | |
| CN103554400A (en) | Liquefaction method of lignin for preparing thermoplastic phenolic resin | |
| CN103588942B (en) | High Performance Phenolic Resins composition and method of making the same | |
| CN112410002B (en) | Cross-linking agent and preparation method thereof, high-temperature delay profile control agent and preparation method thereof | |
| CN108676321A (en) | The method that polyvinyl butyral is modified magnesium phenolic aldehyde is prepared based on solid formaldehyde | |
| CN109535359A (en) | A method of alkali resistance phenolic resin is synthesized based on control solution ph | |
| CN103880611B (en) | A kind of preparation method of bis-hydroxypropyl bisphenol fluorene ether | |
| CN103467682B (en) | Process for circularly producing thermoplastic barium sulfate phenolic resin by precipitation method | |
| CN104164051A (en) | Toughening-type environmental protection phenolic resin and preparation method of its composite material | |
| CN101423593B (en) | Anhydrous phenol formaldehyde resin and production method thereof | |
| CN103193946B (en) | Method for synthesizing base resin by utilizing humic acid | |
| CN103450263A (en) | Preparation method of phosphorus-modified phenolic resin | |
| CN102050534B (en) | Method for treating waste water from rubber antioxidant tmq (RD) device | |
| CN113105638B (en) | Lignin degradation product-bisphenol A-polyurethane polycondensate additive and preparation method thereof | |
| CN110511337A (en) | A method of water soluble phenol resin is prepared using the waste water of production phenolic resin | |
| CN104418530A (en) | Preparation method of ethyl formate composite antifreeze agent | |
| CN104497288A (en) | Alkyd resin and preparation method thereof | |
| CN103450427A (en) | Phosphorus-modified phenolic resin and preparation method thereof | |
| CN103467685A (en) | Phosphorus modified phenolic resin and preparation method thereof | |
| CN103450264A (en) | Preparation method of phosphorus-modified 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 | ||
| WW01 | Invention patent application withdrawn after publication |
Application publication date: 20181019 |
|
| WW01 | Invention patent application withdrawn after publication |