CN109851736A - A kind of preparation method of no nitrogen furan resin - Google Patents
A kind of preparation method of no nitrogen furan resin Download PDFInfo
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- CN109851736A CN109851736A CN201910007835.2A CN201910007835A CN109851736A CN 109851736 A CN109851736 A CN 109851736A CN 201910007835 A CN201910007835 A CN 201910007835A CN 109851736 A CN109851736 A CN 109851736A
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Abstract
The invention discloses a kind of preparation methods of no nitrogen furan resin, it belongs to furane resins production technical field, comprising the following steps: solid formaldehyde and furfuryl alcohol are added in reaction kettle, are stirred, being adjusted with acid pH value is 4.5-6；Catalyst acetic acid zinc is added under above-mentioned acid condition, catalysis reaction is carried out at 130-150 DEG C, constant temperature 3-5 hours, obtains polymer；Aldehyde remover, coupling agent is added, is uniformly mixed；PH value is adjusted to neutrality with sodium hydroxide solution, and blowing obtains product after continuing stirring.By weight, the parts by weight of the raw material of above-mentioned each stage of reaction are as follows: 5-9 parts of solid formaldehyde, 95-100 parts of furfuryl alcohol, 0.2-0.5 parts of zinc acetate, 6-10 parts of aldehyde remover, 0.4-0.8 parts of coupling agent.The present invention obtains that nitrogen-free, low content of free formaldehyde, cost is relatively low, energy conservation and environmental protection, the higher no nitrogen furan resin of intensity by improving raw material and production technology, can be directly used for the production of steel-casting.
Description
Technical field
The present invention relates to furane resins production technical fields, and in particular to a kind of preparation method of no nitrogen furan resin.
Background technique
Furane resins since the 1970s, by nearly popularization in 30 years, are used widely in China.No
It crosses, produces, in China using more mature or nitrogenous furane resins, it is mainly used for Steel Castings, this is because
Wherein contain the reason of more nitrogen, the generation for the defects of nitrogen can cause stomata in steel-casting, nitrogenous furane resins are uncomfortable
Together in Steel Castings, especially large-scale steel-casting and alloy steel casting, with the increasingly raising required casting quality, it is necessary to
Using low nitrogen or the furane resins of nitrogen-free.However, the production without nitrogen furan resin always exists, viscosity is big, free formaldehyde is high, anti-
The low disadvantage of tensile strength, so that production environment is severe in Foundry Production, resin amount is more, and gas forming amount is big, causes
Casting flaw.To hinder application of the furan resin-sand technique in China's Steel Castings.
Summary of the invention
For above-mentioned technical problem, the present invention provides a kind of preparation method of no nitrogen furan resin, by improve raw material and
Production technology, obtains that nitrogen-free, low content of free formaldehyde, cost is relatively low, energy conservation and environmental protection, the higher no nitrogen furan resin of intensity, can be direct
Production for steel-casting.
To achieve the goals above, The technical solution adopted by the invention is as follows:
A kind of preparation method of no nitrogen furan resin, comprising the following steps:
(1) solid formaldehyde and furfuryl alcohol are added in reaction kettle, are stirred, being adjusted with acid pH value is 4.5-6；
(2) catalyst acetic acid zinc is added under above-mentioned acid condition, catalysis reaction, constant temperature 3-5 are carried out at 130-150 DEG C
Hour, obtain polymer；
(3) aldehyde remover, coupling agent is added, is uniformly mixed；
(4) pH value is adjusted to neutrality with sodium hydroxide solution, blowing obtains product after continuing stirring.
By weight, the parts by weight of the raw material of above-mentioned each stage of reaction are as follows: 5-9 parts of solid formaldehyde, furfuryl alcohol 95-
100 parts, 0.2-0.5 parts of zinc acetate, 6-10 parts of aldehyde remover, 0.4-0.8 parts of coupling agent.
Preferably, by weight, the parts by weight of the raw material of above-mentioned each stage of reaction are as follows: 7 parts of solid formaldehyde, furfuryl alcohol
98 parts, 0.3 part of zinc acetate, 8 parts of aldehyde remover, 0.6 part of coupling agent.
Preferably, the solid formaldehyde is the paraformaldehyde of low polymerization degree, content 90.0-99.9%.
Preferably, the coupling agent is N- (β-aminoethyl)-γ-aminopropyltriethoxy dimethoxysilane.
Preferably, the acid in the step (1) is the acetum of concentration 10%.
Preferably, the concentration of sodium hydroxide solution in the step (4) is 20-30%.
Beneficial effects of the present invention are shown: the mild safety of reaction is not easy gel solidification, the Resin Flow being prepared
Good, gel solidification speed is fast, is not dehydrated, and no waste water generates, safety and environmental protection.
The preparation principle of furane resins is made by the hydroxymethylation of furfuryl alcohol and formaldehyde, and reaction product is double hydroxyl first
Base furans, catalyst play crucial effect during the reaction, and traditional catalyst acidic catalyst selects hydrochloric acid, oxalic acid etc.,
Basic catalyst selects piece alkali etc., meets the needs of synthesis to a certain extent, but is the abundant progress of the guarantee reaction, must
Reasonable catalyst must be selected, the present invention in acid condition, uses zinc acetate for catalyst, and it is solid that gel is not easy in reaction process
Change, the Resin Flow being prepared is good, and gel solidification speed is fast；Coupling agent is added in preparation process, obtains the intensity of resin
It is improved to great；Nitrogen is not contained in raw material, nitrogen content is can obviously reduce, substantially reduces damage of the stomata to casting,
It can be directly used for Steel Castings；Liquid formaldehyde is replaced using solid formaldehyde, original can be chemically more advantageous in kinetics
The abundant reaction of material can effectively reduce the reaction time, and replace liquid formaldehyde using solid formaldehyde, reach residual after reduction is reacted
The free formaldehyde content stayed realizes that the target of technical standard can also be reached by exempting from dehydration, to keep product free formaldehyde lower, furthermore
By the way that aldehyde remover is added, free formaldehyde is further decreased, the injury to environment and worker is substantially reduced.
Specific embodiment
In order to facilitate the understanding of those skilled in the art, the present invention is further illustrated combined with specific embodiments below:
Embodiment 1:
A kind of preparation method of no nitrogen furan resin, comprising the following steps:
(1) solid formaldehyde and furfuryl alcohol are added in reaction kettle, are stirred, being adjusted with acid pH value is 4.5-6；
(2) catalyst acetic acid zinc is added under above-mentioned acid condition, catalysis reaction, constant temperature 3-5 are carried out at 130-150 DEG C
Hour, obtain polymer；
(3) aldehyde remover, coupling agent is added, is uniformly mixed；
(4) pH value is adjusted to neutrality with sodium hydroxide solution, blowing obtains product after continuing stirring.
By weight, the parts by weight of the raw material of above-mentioned each stage of reaction are as follows: 7 parts of solid formaldehyde, 98 parts of furfuryl alcohol, second
0.3 part of sour zinc, 8 parts of aldehyde remover, 0.6 part of coupling agent.
The solid formaldehyde is the paraformaldehyde of low polymerization degree, content 90.0-99.9%.The coupling agent is N- (β-
Aminoethyl)-γ-aminopropyltriethoxy dimethoxysilane.Acid in the step (1) is the acetum of concentration 10%.It is described
Concentration of sodium hydroxide solution in step (4) is 20-30%.
Embodiment 2:
A kind of preparation method of no nitrogen furan resin, comprising the following steps:
(1) solid formaldehyde and furfuryl alcohol are added in reaction kettle, are stirred, being adjusted with acid pH value is 4.5-6；
(2) catalyst acetic acid zinc is added under above-mentioned acid condition, catalysis reaction, constant temperature 3-5 are carried out at 130-150 DEG C
Hour, obtain polymer；
(3) aldehyde remover, coupling agent is added, is uniformly mixed；
(4) pH value is adjusted to neutrality with sodium hydroxide solution, blowing obtains product after continuing stirring.
By weight, the parts by weight of the raw material of above-mentioned each stage of reaction are as follows: 5 parts of solid formaldehyde, 95 parts of furfuryl alcohol, second
0.2 part of sour zinc, 6 parts of aldehyde remover, 0.4 part of coupling agent.
The solid formaldehyde is the paraformaldehyde of low polymerization degree, content 90.0-99.9%.The coupling agent is N- (β-
Aminoethyl)-γ-aminopropyltriethoxy dimethoxysilane.Acid in the step (1) is the acetum of concentration 10%.It is described
Concentration of sodium hydroxide solution in step (4) is 20-30%.
Embodiment 3:
A kind of preparation method of no nitrogen furan resin, comprising the following steps:
(1) solid formaldehyde and furfuryl alcohol are added in reaction kettle, are stirred, being adjusted with acid pH value is 4.5-6；
(2) catalyst acetic acid zinc is added under above-mentioned acid condition, catalysis reaction, constant temperature 3-5 are carried out at 130-150 DEG C
Hour, obtain polymer；
(3) aldehyde remover, coupling agent is added, is uniformly mixed；
(4) pH value is adjusted to neutrality with sodium hydroxide solution, blowing obtains product after continuing stirring.
By weight, the parts by weight of the raw material of above-mentioned each stage of reaction are as follows: 9 parts of solid formaldehyde, 100 parts of furfuryl alcohol,
0.5 part of zinc acetate, 10 parts of aldehyde remover, 0.8 part of coupling agent.
The solid formaldehyde is the paraformaldehyde of low polymerization degree, content 90.0-99.9%.The coupling agent is N- (β-
Aminoethyl)-γ-aminopropyltriethoxy dimethoxysilane.Acid in the step (1) is the acetum of concentration 10%.It is described
Concentration of sodium hydroxide solution in step (4) is 20-30%.
Above content is only to structure example of the invention and explanation, affiliated those skilled in the art
It makes various modifications or additions to the described embodiments or is substituted in a similar manner, without departing from invention
Structure or beyond the scope defined by this claim, be within the scope of protection of the invention.
Claims (6)
1. a kind of preparation method of no nitrogen furan resin, which comprises the following steps:
(1) solid formaldehyde and furfuryl alcohol are added in reaction kettle, are stirred, being adjusted with acid pH value is 4.5-6；
(2) catalyst acetic acid zinc is added under above-mentioned acid condition, catalysis reaction is carried out at 130-150 DEG C, constant temperature 3-5 is small
When, obtain polymer；
(3) aldehyde remover, coupling agent is added, is uniformly mixed；
(4) pH value is adjusted to neutrality with sodium hydroxide solution, blowing obtains product after continuing stirring；
By weight, the parts by weight of the raw material of above-mentioned each stage of reaction are as follows: 5-9 parts of solid formaldehyde, 95-100 parts of furfuryl alcohol,
0.2-0.5 parts of zinc acetate, 6-10 parts of aldehyde remover, 0.4-0.8 parts of coupling agent.
2. a kind of preparation method of no nitrogen furan resin according to claim 1, which is characterized in that by weight, on
State the parts by weight of the raw material of each stage of reaction are as follows: 7 parts of solid formaldehyde, 98 parts of furfuryl alcohol, 0.3 part of zinc acetate, 8 parts of aldehyde remover,
0.6 part of coupling agent.
3. a kind of preparation method of no nitrogen furan resin according to claim 1, which is characterized in that the solid formaldehyde is
The paraformaldehyde of low polymerization degree, content 90.0-99.9%.
4. a kind of preparation method of no nitrogen furan resin according to claim 1, which is characterized in that the coupling agent is N-
(β-aminoethyl)-γ-aminopropyltriethoxy dimethoxysilane.
5. a kind of preparation method of no nitrogen furan resin according to claim 1, which is characterized in that in the step (1)
Acid be concentration 10% acetum.
6. a kind of preparation method of no nitrogen furan resin according to claim 1, which is characterized in that in the step (4)
Concentration of sodium hydroxide solution be 20-30%.
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| CN201910007835.2A CN109851736A (en) | 2019-01-04 | 2019-01-04 | A kind of preparation method of no nitrogen furan resin |
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| CN201910007835.2A CN109851736A (en) | 2019-01-04 | 2019-01-04 | A kind of preparation method of no nitrogen furan resin |
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| CN109851736A true CN109851736A (en) | 2019-06-07 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114920895A (en) * | 2022-06-23 | 2022-08-19 | 山东永创材料科技有限公司 | Preparation method of cold-resistant furan resin |
-
2019
- 2019-01-04 CN CN201910007835.2A patent/CN109851736A/en not_active Withdrawn
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114920895A (en) * | 2022-06-23 | 2022-08-19 | 山东永创材料科技有限公司 | Preparation method of cold-resistant furan resin |
| CN114920895B (en) * | 2022-06-23 | 2023-09-29 | 山东永创材料科技有限公司 | Preparation method of cold-resistant furan resin |
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Application publication date: 20190607 |