CN1074802C - Method for making low-viscosity stable aminoresin initial reduced body - Google Patents
Method for making low-viscosity stable aminoresin initial reduced body Download PDFInfo
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- CN1074802C CN1074802C CN97119755A CN97119755A CN1074802C CN 1074802 C CN1074802 C CN 1074802C CN 97119755 A CN97119755 A CN 97119755A CN 97119755 A CN97119755 A CN 97119755A CN 1074802 C CN1074802 C CN 1074802C
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Abstract
The present invention relates to an organic compound for treating fibers, yarn, threads, fabrics or fiber products thereof. The organic compound is made by the following method: 100 parts by weight of formaldehyde, 3 to 15 parts by weight of melamine, 20 to 40 parts by weight of urea and 0.1 to 0.2 part by weight of organic acid are put into a reaction vessel to be stirred; when the temperature in the reaction vessel increases to 36 to 48 DEG C, riethylamine is used to regulate the pH value of the components to 8 to 9; 30 to 50 parts by weight of urea is added to the components to obtain a mixture; water is added to the mixture to adjust the solid content of the mixture to be less than 55%; the mixture is cooled and then discharged. The method is characterized in that the proportion of the formaldehyde to amino substances is controlled to effectively prevent the generation of polymers; reaction is carried out at normal temperature, and stable amine resin initial condensate with hypoviscosity can be obtained without adding alcohol for etherification. The product of the compound finishes textiles easily.
Description
The present invention relates to a kind ofly be used to handle fiber, yarn, line, fabric or by the organic compound of its fibre of making.
The water soluble amino resin initial reduced body can be used for fabric is carried out RESIN FINISH, makes fabric have anti-water or flame-retarding characteristic.At present, general water soluble amino resin initial reduced body all is synthesized into by formaldehyde and urea, melamine, its synthetic method is finished by two steps, at first allow formaldehyde and melamine, urea polymerization, and then allow the methylolurea or the melamine methylol of polymerisation generation change into methoxy urea or methoxy three polyoxy amine with methanol-ethers again, its process is as follows:
In first step course of reaction,, make initial reduced body instability and viscosity increase the sky, the arrangement of unfavorable fabric if the ratio of formaldehyde molal quantity and amino group molal quantity less than 1, then is easy to generate polymer in the process of synthetic initial reduced body.In addition, the temperature of etherification procedure is higher, if there is not methylolated amino in the system, then easy and methylol further generates poly or high polymer, and initial reduced body viscosity increases and is unstable.Therefore, the mole ratio of formaldehyde and urea or formaldehyde and melamine is respectively greater than 2 or 3.And such gram molecule proportioning, free content of formaldehyde is big in the system, and the formaldehyde that fabric is overflowed when arrangement bakes is many, smell is dense, harmful health.Entire reaction also must be transferred pH value (make and be alkalescence), heating, cooling.And when fabric is carried out RESIN FINISH, need to bake with higher temperature, its ehter bond is disconnected, emit methyl alcohol or ethanol again, polycondensation forms the strong high polymer of hydrophobicity again.
Tongan City resin that the East Sea, Shanghai aquatic products research institute produces is used for the textile finishing to nylon terylene fishing net, paper industry guipure, its prescription way is: formaldehyde is 100 parts by weight, 30 parts in urea, 5 parts of melamines, 5 parts of ethanol, i.e. heating after feeding intake, be warming up to 75～77 ℃, adding 1.5 parts of accent of triethanolamine pH value rapidly is 8～9, adds 20 parts in urea again, and be cooled to rapidly below 40 ℃, make product rejection if often occur poly-cruelly under failing in 60 minutes, to be chilled to 40 ℃.This production method not only need add pure etherificate, and the difficult grasp of reaction condition.
The purpose of this invention is to provide a kind of reaction at normal temperatures, needn't add the manufacture method that the alcohols etherificate can obtain low-viscosity stable aminoresin initial reduced body.
Concrete grammar of the present invention is as follows.Get 100 parts in 37% formaldehyde at first by weight ratio, 3～15 parts of melamines, 20～40 parts in urea, other adds organic acid and makes catalyst for 0.1～0.2 part, said organic acid is a formic acid, citric acid or phthalate anhydride, can stir after adding reactor, follow the endothermic process of material dissolution when initial, temperature sharply descends, thereafter the exothermic heat of reaction temperature recovery, when treating that temperature rises to 36～48 ℃, regulating pH value with triethanolamine is 8～9, adds 20～50 parts in urea again, adds water and regulates solid content (55%, naturally cooling just can obtain stable low viscosity aminoresin initial reduced body.
Characteristics of the present invention are proportionings of control formaldehyde and amino material, and the mole ratio that makes formaldehyde and amino material can effectively stop the generation of high polymer much smaller than 2 (1.7～1.0).In addition, entire reaction stirs at normal temperatures carries out, and the control temperature rise needn't add pure etherificate and can obtain low viscosity (3～8mPaS) stable aminoresin initial reduced bodies.With this initial reduced body fabric is put in order, need not be baked by high temperature, only need oven for drying, can obtain satisfied finishing effect at 70～95 ℃.Simultaneously by adjusting content of urea, can make fabric have anti-water, crease-resistant or fire-retardant characteristic.In addition, in operating process, do not have harmful formaldehyde odor (general content of formaldehyde be lower than 0.5%), and content of formaldehyde is 2% when preparing with other method.
The present invention is further illustrated below by embodiment.
Embodiment 1: get 37% formaldehyde 100Kg, melamine 5Kg, urea 30Kg, formic acid 100g, stir after dropping into reactor, initial temperature sharply descends, thereafter go up, when treating that temperature rises to 40～41 ℃, add triethanolamine 1.5Kg, add 30Kg urea, 30Kg water again, can stop to stir discharging behind the 20min.With this resin initial reduced body fabric is put in order, the anti-water wrinkle resistance of fabric improves greatly.
Embodiment 2: get 37% formaldehyde 100Kg, melamine 6Kg, urea 25Kg, phthalate anhydride 120g drops into reactor and promptly stirs.Identical with the process of example 1, when Te Wendu rises to 42～43 ℃, add triethanolamine 1.5Kg, urea 20Kg, water 20Kg.Get final product discharging behind the 20min.The resin liquid initial reduced body and the example 1 of gained are similar.
Embodiment 3: get 37% formaldehyde 100Kg, melamine 4Kg, urea 25Kg, citric acid 120g.With example 1 identical way, when Te Wendu rises to 42～43 ℃, add triethanolamine 1.5Kg, urea 45Kg, water 50Kg.Stop behind the 20min stirring.This resin initial reduced body nitrogen content is higher, can cooperate fabric to do the flame-retarded resin arrangement.
Embodiment 4～6: its step and embodiment 1～3 are similar, its prescription, proportioning and process conditions such as following table.Real 37% 3 urea (Kg) lemon adds Shi Jiaju fully--lemon T water example aldehyde cyanogen M acid amount
Amine one or two is annotated
(Kg) (Kg) inferior (g) (℃) (Kg) 4 100 3 40 10 1.53 105 36 30 be used for the anti-water of fabric and put 5 100 15 20 20 1.67 100 40 35 in order and be used for the anti-water of fabric and put 6 100 4 30 50 1.0 200 48 40 in order and be used for fabric fire-retardant finishing
Annotate: 1.M is the mole ratio of formaldehyde and amino material.
2.T for transferring the temperature of pH value to 8～9.
Claims (2)
1. the manufacture method of low-viscosity stable aminoresin initial reduced body, carry out synthetic reaction by formaldehyde, melamine, urea, it is characterized in that getting at first by weight ratio 100 parts in 37% formaldehyde, 3～15 parts of melamines, 20～40 parts in urea, other adds 0.1～0.2 part of organic acid, stirs after adding reactor, when treating temperature to 36～48 ℃, regulating pH value with triethanolamine is 8～9, add 20～50 parts in urea again, add water and regulate solid content＜55%, cooling back discharging naturally.
2. the manufacture method of low-viscosity stable aminoresin initial reduced body as claimed in claim 1 is characterized in that said organic acid is formic acid, citric acid or phthalate anhydride.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN97119755A CN1074802C (en) | 1997-10-21 | 1997-10-21 | Method for making low-viscosity stable aminoresin initial reduced body |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN97119755A CN1074802C (en) | 1997-10-21 | 1997-10-21 | Method for making low-viscosity stable aminoresin initial reduced body |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1215107A CN1215107A (en) | 1999-04-28 |
| CN1074802C true CN1074802C (en) | 2001-11-14 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN97119755A Expired - Fee Related CN1074802C (en) | 1997-10-21 | 1997-10-21 | Method for making low-viscosity stable aminoresin initial reduced body |
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| Country | Link |
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| CN (1) | CN1074802C (en) |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN86107140A (en) * | 1985-10-23 | 1987-04-29 | 第一工业制药株式会社 | The resin treatment method of the textiles of cellulose fiber |
-
1997
- 1997-10-21 CN CN97119755A patent/CN1074802C/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN86107140A (en) * | 1985-10-23 | 1987-04-29 | 第一工业制药株式会社 | The resin treatment method of the textiles of cellulose fiber |
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| Publication number | Publication date |
|---|---|
| CN1215107A (en) | 1999-04-28 |
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