CN109608602A - High activity environment-friendly type flower mud phenolic resin and preparation method thereof - Google Patents
High activity environment-friendly type flower mud phenolic resin and preparation method thereof Download PDFInfo
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- CN109608602A CN109608602A CN201811412858.3A CN201811412858A CN109608602A CN 109608602 A CN109608602 A CN 109608602A CN 201811412858 A CN201811412858 A CN 201811412858A CN 109608602 A CN109608602 A CN 109608602A
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- phenolic resin
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- high activity
- friendly type
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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
- C08G14/00—Condensation polymers of aldehydes or ketones with two or more other monomers covered by at least two of the groups C08G8/00 - C08G12/00
- C08G14/02—Condensation polymers of aldehydes or ketones with two or more other monomers covered by at least two of the groups C08G8/00 - C08G12/00 of aldehydes
- C08G14/04—Condensation polymers of aldehydes or ketones with two or more other monomers covered by at least two of the groups C08G8/00 - C08G12/00 of aldehydes with phenols
- C08G14/06—Condensation polymers of aldehydes or ketones with two or more other monomers covered by at least two of the groups C08G8/00 - C08G12/00 of aldehydes with phenols and monomers containing hydrogen attached to nitrogen
- C08G14/08—Ureas; Thioureas
Abstract
The present invention provides high activity environment-friendly type flower mud phenolic resin, raw material includes phenol, paraformaldehyde, formaldehyde, pH adjusting agent, urea, formic acid and ethylene glycol.The present invention also provides the preparation methods of above-mentioned phenolic resin.High activity environment-friendly type flower mud phenolic resin provided by the invention, the brittleness of phenol formaldehyde foam is utilized, percent opening is high, and water imbibition is strong, and water retention property is good, suitable for production flower mud, phenol formaldehyde foam is made with phenolic resin using high activity environment-friendly type flower mud provided by the invention, in the phenol formaldehyde foam that fresh flower insertion is sufficiently absorbed water, can significantly extend the service life of fresh flower, enhancing flower arrangement or the beautification of the gaily decorated basket and appreciation effect, it is fresh-keeping for the fresh flower of long-distance transport more to have special value.
Description
Technical field
The invention belongs to technical field of polymer materials, and in particular to high activity environment-friendly type flower mud phenolic resin and its system
Preparation Method.
Background technique
In recent years, since the heat of skyscraper, communications and transportation, aircraft industry, space technology etc. to synthetic foam is steady
Qualitative and flame resistance proposes tightened up requirement, also rapidly develops phenol formaldehyde foam.Phenol formaldehyde foam is a kind of
Cheap and good-quality light heat-insulating material, is suitable as construction material, with light-weight, thermal insulation is good, rigidity is big and dimensionally stable
The good feature of property.Phenol formaldehyde foam has the coefficient of expansion similar with aluminium, will not melt when being also equipped with burning, object, low hair without dripping off
The characteristic of smoke, and carbon monoxide toxic gas is not generated in burning.As a kind of novel multi-purpose foam material, phenol
Aldehyde foam penetrates with its heat resistance, fire retardant self-extinguishment, flame resistant, the advantages that meeting fire without dripping off and it is in widespread attention.
The preparation process of phenol formaldehyde foam is to fill phenolic resin and surfactant, foaming agent, curing agent and other auxiliary agents
Divide after being mixed, then this mixture is poured into mold, phenolic resin crosslinking curing under the promotion of curing agent is released simultaneously
Heat, the heat promote foaming agent to vaporize and form micropore in mixture, form phenol formaldehyde foam by the regular hour.
CN102731740B discloses a kind of method with paraformaldehyde production expandable phenolic resin, and step prepares raw material phenol, more
Polyformaldehyde, base catalyst, urea and diluent, then raw material is reacted in a kettle under normal pressure, at 55 DEG C -90 DEG C, the party
Method solves the problems, such as formaldehyde heat release, ensure that the whole uniformity of product.CN103819638B discloses a kind of low viscosity can
Hair property phenolic resin and preparation method thereof, raw material includes phenol, paraformaldehyde, sodium hydroxide, barium hydroxide, diluent, urea
And inorganic fillings, the invention use sodium hydroxide and barium hydroxide compounded catalyst substep catalytic degradation and polycondensation reaction,
Cooperate diluent cooling, letdown resin viscosity, solve paraformaldehyde expandable phenolic resin production, it is excessive using medium viscosity
Problem, the phenolic resin viscosity is low, and good flame resistance, manufacturing cost is low, and preparation method is simple and easy to control, stable reaction, rate be high,
Yield is high, high-quality, and no sudden and violent kettle, plug casting machine hidden danger produce, using safe.
With economic development, social progress and the improvement of people's living standards, the application of fresh flower is gradually from hotel, meal
Daily life, Bu Ren common people family are come into the places such as shop, meeting-place.Flower mud is that a kind of flower material applied to flower arrangement creation is solid
Material is determined, for fine and closely woven porous spongy foam body, with high water imbibition, high-moisture-retention, quality is crisp and has one
Fixed mechanical strength plays a part of extending fresh flower freshness date, therefore, is liked by flower arrangement fan and fresh flower operator.
The raw material that can be used for making flower mud has phenolic aldehyde (PF) resin, ureaformaldehyde (UF) resin, polyurethane (Pu) resin etc., but due to polyurethane
The reasons such as resin raw material is expensive, and Lauxite intensity is higher, and scape is not easy to be inserted into seldom use.
Phenolic resin has the fundamental characteristics for being made into flower mud because of its characteristic.However, because of reactive modified phenolic resin speed
Degree is fast, requires harshness to reaction condition, exists with the phenolic foam resin that the furnished equipments such as the common reaction kettle of current chemical industry go out
Molecular weight, activity, viscosity equistability are poor, and free formaldehyde is high, it is difficult to normalization industrial production, the dedicated thermosetting phenolic of flower mud
Resin is not yet mature, is only replaced with the phenolic foam resin of building thermal insulation material, and building thermal insulation material phenolic foam
Resin is because reactivity is poor, and percent opening is low after foaming, expansion ratio is low, at high cost, and it is many as flower mud product defect.Cause
This, still needs to develop a kind of new flower mud phenolic resin.
Summary of the invention
To solve problems of the prior art, one of the objects of the present invention is to provide a kind of high activity environment-friendly type flowers
Mud phenolic resin.
The second object of the present invention is to provide the preparation method of above-mentioned high activity environment-friendly type flower mud phenolic resin.
High activity environment-friendly type flower mud phenolic resin, raw material include the component of following parts by weight meter:
40~55 parts of phenol,
20~40 parts of paraformaldehyde,
2~10 parts of formaldehyde,
1~5 part of pH adjusting agent,
5~15 parts of urea,
0.5~4 part of formic acid,
5~15 parts of ethylene glycol.
Preferably, raw material includes the component of following parts by weight meter:
40~55 parts of phenol,
24~36 parts of paraformaldehyde,
3~7 parts of formaldehyde,
1~3.5 part of pH adjusting agent,
6~11 parts of urea,
0.5~2.5 part of formic acid,
6.5~10 parts of ethylene glycol.
Preferably, the mass percent concentration of the formaldehyde is 37%.
Preferably, the pH adjusting agent is sodium hydroxide.
It is further preferred that the mass percent concentration of the sodium hydroxide is 30~50%.
The preparation method of above-mentioned high activity environment-friendly type flower mud phenolic resin, step include:
(1) each component is weighed according to the ratio, and pH adjusting agent is divided into 3 parts；
(2) reaction kettle is added in the phenol, paraformaldehyde and formaldehyde, first part of pH adjusting agent of addition after stirring, first
90~120min is reacted after secondary heating；
(3) second part of pH adjusting agent is added into the reaction kettle of step (2), reacts 30~60min after second of heating；
(4) third part pH adjusting agent is added into the reaction kettle of step (3), third time is reacted 30~60min after heating up, taken
Sample detects the water solubility of phenolic resin, and urea is added when reaching 300~400% in water solubility, the reaction was continued to it is water-soluble it is up to standard after
Formic acid is added；
(5) ethylene glycol is added after cooling down.
Preferably, the mass ratio of first part of pH adjusting agent, second part of pH adjusting agent and third part pH adjusting agent is 2:
1:1.
Preferably, the temperature of step (2) the first time heating is 45~60 DEG C；Step (3) second of heating
Temperature is 60~75 DEG C；The temperature of step (4) the third time heating is 75~90 DEG C.
Preferably, step (4) water solubility up to standard is 200~300%.
Preferably, water-soluble detection method are as follows: weigh 10 grams of resins, resin is neutralized to neutrality, is titrated with distilled water, is arrived
Ml of consumption water is accurately read when muddy, reading is water-soluble numerical value divided by 10.
In preparation method, substep puts into the effect of sodium hydroxide in addition to controlling heating rate, and there are also two aspect effects, first is that
It is easy to operate, it is conducive to stability contorting and reacts, is all to put into paraformaldehyde by several times mostly, however because of poly first in the prior art
Aldehyde smell is big, is solid, and repeatedly investment paraformaldehyde is inconvenient, and investment may require that longer time, influence reaction temperature, right
Stability contorting reaction has adverse effect；Second is that substep be added sodium hydroxide, can substep addition reaction, conducive to the methylol of phenol
Change, is conducive to resin activity.
The brittleness of phenol formaldehyde foam is utilized in high activity environment-friendly type flower mud phenolic resin, while percent opening is high, imparts it
Fresh flower is inserted into the phenol formaldehyde foam sufficiently to absorb water by sufficient water imbibition, can greatly prolong the service life of fresh flower, enhancing flower arrangement or flower
The beautification and appreciation effect of basket, fresh-keeping for the fresh flower of long-distance transport more have special value.
Beneficial effects of the present invention
1, high activity environment-friendly type flower mud phenolic resin provided by the invention, free formaldehyde content is compared under the usual products of market
Drop is obvious, and average down ratio is 61.9%, and environmental-protecting performance is obviously improved, and viscosity average specific usual products reduce by 41.3%, hair
Heat average specific usual products increase 101.2%, meet the requirement of flower mud phenolic foam resin high activity, are suitable for
Produce flower mud；
2, phenol formaldehyde foam is made with phenolic resin using high activity environment-friendly type flower mud provided by the invention, fresh flower insertion is filled
Divide in the phenol formaldehyde foam of water suction, can significantly extend the service life of fresh flower, enhance flower arrangement or the beautification of the gaily decorated basket and appreciate effect, for length
The fresh flower of way transport is fresh-keeping more special value；
3, preparation method of phenolic resin of the invention is added sodium hydroxide by gradation, heating rate is controlled, using centre
Control means precisely determine the terminal of reaction, have reached and stably produced high activity, high-precision requirement with the equipment of simple general-purpose
Phenolic foam resin purpose, entire production process exempt from dehydration, without waste water and gas discharge, product free formaldehyde significantly reduce,
It is environmental-friendly；
4, in preparation method, the effect of sodium hydroxide is put into step by step in addition to controlling heating rate, there are also two aspects to act on, and one
Be it is easy to operate, be conducive to stability contorting and react, be all to put into paraformaldehyde by several times mostly, however because of poly in the prior art
Formaldehyde odor is big, is solid, and repeatedly investment paraformaldehyde is inconvenient, and investment may require that longer time, influences reaction temperature,
There is adverse effect to stability contorting reaction；Second is that substep be added sodium hydroxide, can substep addition reaction, conducive to the hydroxyl first of phenol
Base is conducive to resin activity.
Specific embodiment
The following is specific embodiments of the present invention, and further retouches to technical solution of the present invention work in conjunction with the embodiments
It states, however, the present invention is not limited to these examples.
Embodiment 1
High activity environment-friendly type flower mud phenolic resin, raw material include the component of following parts by weight meter:
40 parts of phenol, 20 parts of paraformaldehyde, 2 parts of formaldehyde, 1 part of pH adjusting agent, 5 parts of urea, 0.5 part of formic acid, ethylene glycol 5
Part.
Embodiment 2
High activity environment-friendly type flower mud phenolic resin, raw material include the component of following parts by weight meter:
55 parts of phenol, 40 parts of paraformaldehyde, 10 parts of formaldehyde, 5 parts of pH adjusting agent, 15 parts of urea, 4 parts of formic acid, ethylene glycol 15
Part.
Embodiment 3
High activity environment-friendly type flower mud phenolic resin, raw material include the component of following parts by weight meter:
45 parts of phenol, 30 parts of paraformaldehyde, 6 parts of formaldehyde, 3 parts of pH adjusting agent, 10 parts of urea, 2.5 parts of formic acid, ethylene glycol 10
Part.
Embodiment 4
The preparation method of high activity environment-friendly type flower mud phenolic resin, step include:
(1) each component is weighed according to the ratio, and pH adjusting agent is divided into 3 parts；
(2) reaction kettle is added in the phenol, paraformaldehyde and formaldehyde, first part of pH adjusting agent of addition after stirring, first
90~120min is reacted after secondary heating；
(3) second part of pH adjusting agent is added into the reaction kettle of step (2), reacts 30~60min after second of heating；
(4) third part pH adjusting agent is added into the reaction kettle of step (3), third time is reacted 30~60min after heating up, taken
Sample detects the water solubility of phenolic resin, and urea is added when reaching 300~400% in water solubility, the reaction was continued to it is water-soluble it is up to standard after
Formic acid is added；
(5) ethylene glycol is added after cooling down.
Wherein, the mass ratio of first part of pH adjusting agent, second part of pH adjusting agent and third part pH adjusting agent is 2:1:1.
The temperature of step (2) the first time heating is 45~60 DEG C；The temperature of step (3) second of heating is 60
~75 DEG C；The temperature of step (4) third time heating is 75~90 DEG C, step (4) water solubility up to standard is 200~
300%.
Water-soluble detection method are as follows: weigh 10 grams of resins, resin is neutralized to neutrality, is titrated with distilled water, when arriving muddy
Accurate ml for reading consumption water, reading are water-soluble numerical value divided by 10.
Detect example
The three of corresponding formula number have been prepared according to the method that embodiment 4 provides using the formula of Examples 1 to 3
Kind flower mud phenolic resin, tests the free formaldehyde content of three kinds of phenolic resin, the viscosity of resin and calorific value, in the market
The most common phenolic foam resin is as reference, and the results are shown in Table 1.
1 phenolic resin test result of table
Fever quantity measuring method: 100g resin to be measured and 15g special curing agent are weighed, temperature control, will be dedicated to 25 DEG C respectively
Curing agent is added in resin, is stirred evenly with thermometer rapidly, it is ensured that thermometer is inserted into resin liquid, records one every 30 seconds
Secondary temperature, until temperature reaches peak, record maximum temperature is the calorific value of resin.
Calorific value reflects the activity of resin, and calorific value is bigger, illustrates that resin activity is higher, expansion ratio and percent opening
It is higher, meet to the flower mud requirement of phenolic foam resin.
As shown in Table 1, the high activity environment-friendly type flower mud phenolic foam resin prepared using method provided by the invention, trip
Obvious compared with the common phenolic foam resin decline in market from content of formaldehyde, average down ratio is 61.9%, and environmental-protecting performance obviously changes
It is kind；Viscosity average specific usual products reduce by 41.3%, and the common phenolic foam resin in calorific value average specific market increases
101.2%, solve the requirement of flower mud phenolic foam resin high activity.
Although common phenolic foam resin can be used for production flower mud in the market, because of poor activity, calorific value is low,
If will lead to for flower mud, percent opening is low, expansion ratio is low, water absorbing and retaining properties are poor, fresh flower fresh-keeping effect difference and at high cost asks
Topic, and phenolic resin of the invention is suitble to produce flower mud.
Claims (9)
1. high activity environment-friendly type flower mud phenolic resin, which is characterized in that raw material includes the component of following parts by weight meter:
40~55 parts of phenol,
20~40 parts of paraformaldehyde,
2~10 parts of formaldehyde,
1~5 part of pH adjusting agent,
5~15 parts of urea,
0.4~4 part of formic acid,
5~15 parts of ethylene glycol.
2. high activity environment-friendly type flower mud phenolic resin according to claim 1, which is characterized in that raw material includes following heavy
Measure the component of part meter:
40~55 parts of phenol,
24~36 parts of paraformaldehyde,
3~7 parts of formaldehyde,
1~3.5 part of pH adjusting agent,
6~11 parts of urea,
0.5~2.5 part of formic acid,
6.5~10 parts of ethylene glycol.
3. high activity environment-friendly type flower mud phenolic resin according to claim 1 or 2, which is characterized in that the formaldehyde
Mass percent concentration is 37%.
4. high activity environment-friendly type flower mud phenolic resin according to claim 1 or 2, which is characterized in that the pH is adjusted
Agent is sodium hydroxide.
5. high activity environment-friendly type flower mud phenolic resin according to claim 4, which is characterized in that the sodium hydroxide
Mass percent concentration is 30~50%.
6. the preparation method of any one high activity environment-friendly type flower mud phenolic resin, feature exist according to claim 1~5
In step includes:
(1) each component is weighed according to the ratio, and pH adjusting agent is divided into 3 parts；
(2) reaction kettle is added in the phenol, paraformaldehyde and formaldehyde, first part of pH adjusting agent is added after stirring, rises for the first time
90~120min is reacted after temperature；
(3) second part of pH adjusting agent is added into the reaction kettle of step (2), reacts 30~60min after second of heating；
(4) third part pH adjusting agent is added into the reaction kettle of step (3), third time reacts 30~60min, sampling inspection after heating up
The water solubility of phenolic resin is surveyed, urea is added when reaching 300~400% in water solubility, and the reaction was continued to water-soluble rear addition up to standard
Formic acid；
(5) ethylene glycol is added after cooling down.
7. the preparation method of high activity environment-friendly type flower mud phenolic resin according to claim 6, which is characterized in that described
The mass ratio of a pH adjusting agent, second part of pH adjusting agent and third part pH adjusting agent is 2:1:1.
8. the preparation method of high activity environment-friendly type flower mud phenolic resin according to claim 6, which is characterized in that step
(2) temperature of the first time heating is 45~60 DEG C；The temperature of step (3) second of heating is 60~75 DEG C；Step
(4) temperature of the third time heating is 75~90 DEG C.
9. according to claim 6 according to the preparation method of the high activity environment-friendly type flower mud phenolic resin, which is characterized in that step
Suddenly (4) described water solubility up to standard is 200~300%.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110041479A (en) * | 2019-04-08 | 2019-07-23 | 太尔化工（南京）有限公司 | A kind of preparation of novel super absorbent phenolic aldehyde flower mud resin and application method |
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| CN1071177A (en) * | 1991-12-07 | 1993-04-21 | 中国科学院广州化学所 | The method for making of water-absorbent phenolic foamed plastics |
| CN102766243A (en) * | 2012-07-25 | 2012-11-07 | 胡玉 | Room-temperature foamable phenolic resin and method for preparing phenolic foams by same |
| CN103819638A (en) * | 2013-11-21 | 2014-05-28 | 江苏兆胜建材有限公司 | Low-viscosity expandable phenolic resin and preparation method thereof |
| CN104387540A (en) * | 2014-10-28 | 2015-03-04 | 中国林业科学研究院林业研究所 | Degradable foam composition for seedling raising or flower arrangement, and manufacturing method and application thereof |
| CN105199063A (en) * | 2015-10-28 | 2015-12-30 | 桓台县永汇化工有限公司 | Preparation method for synthesis of phenolic resin from paraformaldehyde |
| CN105837769A (en) * | 2016-05-16 | 2016-08-10 | 华南理工大学 | Low-formaldehyde-emission high-water-solution-multiple high-temperature-resistant phenolic resin and preparation method thereof |
-
2018
- 2018-11-23 CN CN201811412858.3A patent/CN109608602A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5876432A (en) * | 1981-10-30 | 1983-05-09 | Chugoku Kako Kk | Preparation of resol phenolic resin foam having improved water absorbing and retaining property |
| CN1071177A (en) * | 1991-12-07 | 1993-04-21 | 中国科学院广州化学所 | The method for making of water-absorbent phenolic foamed plastics |
| CN102766243A (en) * | 2012-07-25 | 2012-11-07 | 胡玉 | Room-temperature foamable phenolic resin and method for preparing phenolic foams by same |
| CN103819638A (en) * | 2013-11-21 | 2014-05-28 | 江苏兆胜建材有限公司 | Low-viscosity expandable phenolic resin and preparation method thereof |
| CN104387540A (en) * | 2014-10-28 | 2015-03-04 | 中国林业科学研究院林业研究所 | Degradable foam composition for seedling raising or flower arrangement, and manufacturing method and application thereof |
| CN105199063A (en) * | 2015-10-28 | 2015-12-30 | 桓台县永汇化工有限公司 | Preparation method for synthesis of phenolic resin from paraformaldehyde |
| CN105837769A (en) * | 2016-05-16 | 2016-08-10 | 华南理工大学 | Low-formaldehyde-emission high-water-solution-multiple high-temperature-resistant phenolic resin and preparation method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110041479A (en) * | 2019-04-08 | 2019-07-23 | 太尔化工（南京）有限公司 | A kind of preparation of novel super absorbent phenolic aldehyde flower mud resin and application method |
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Address after: No. 2010, Huangyang Avenue, Doumen Town, Doumen District, Zhuhai City, Guangdong Province Applicant after: Guangdong Casting Material Technology Co., Ltd Address before: 519000 Guangdong city in Zhuhai Province town of Doumen District Xinqing Industrial Park Xinqing road six Applicant before: Zhuhai Doumen Fulian Molding Material Industrial Co., Ltd. |
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