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Polymerized rosin derivant, preparing method and uses thereof

A technology for polymerizing rosin and manufacturing methods, applied in the direction of manufacturing tools, adhesive additives, polymer adhesive additives, etc., can solve the restrictions on the use of unsaturated carboxylic acids, residual sulfur components, adhesion, adhesive color, thermal stability Deterioration and other problems, to achieve the effect of good color tone and heating stability, good stability, and good color tone

Inactive Publication Date: 2008-09-24
ARAKAWA CHEM IND LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] However, in the techniques described in Cited Document 1 and Cited Document 2, the high-yield methods all use acidic catalysts such as sulfuric acid, and therefore there is a problem that the catalyst or the decomposition of the catalyst remains in the obtained resin. Sulfur components caused by substances (refer to Table 1 of Patent Document 2)
[0012] In addition, the colorless polymerized rosin obtained by the methods described in Cited Document 3 and Cited Document 4 has problems such as being unable to be modified by unsaturated carboxylic acid and the like due to hydrogenation or disproportionation, and thus limited in use.
Also, these methods are to refine the rosin, polymerize it, esterify it, and then hydrogenate it. If the polymerized rosin is prepared in advance and used after long-term storage, the color may not be sufficiently lightened. the situation happened
If such a polymerized rosin is used, the color tone and thermal stability of the adhesive / adhesive deteriorate, so there is a problem that the appearance is damaged, and improvement is required

Method used

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  • Polymerized rosin derivant, preparing method and uses thereof
  • Polymerized rosin derivant, preparing method and uses thereof
  • Polymerized rosin derivant, preparing method and uses thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0090] (1) refined

[0091] An unrefined rosin (resin rosin produced in China) with an acid value of 170.0 mg KOH / g, a softening point of 78°C, and a hue of Gardner 6 was distilled under a nitrogen seal at a reduced pressure of 400 Pa, and the main fraction shown in Table 1 was determined as Refined Rosin. The acid value of this purified rosin was 178.4 mg KOH / g, the softening point was 88°C, and the hue (Gardner color value) was 3.

[0092] 【Table 1】

[0093] Outflow temperature (°C)

Kettle temperature

yield

Acid value (mg / KOH)

[0094] (℃)

(％)

initial fraction

Less than 195

Less than 210

4.4

51.2

main fraction

195～250

210～280

88.2

178.4

Residue in kettle

more than 250

more than 280

7.4

45.6

[0095] (2) Polymerization reaction

[0096] In the reaction device with thermometer, stirrer, nitrogen inlet pipe and decompression device...

Embodiment 2

[0100] In the autoclave reaction device, load the desulfurization refining polymerized rosin 150g obtained by embodiment 1, palladium carbon (water content 50%) 1.5g and hexanaphthene 150g as the hydrogenation catalyst, remove the oxygen in the system, use Pressurize the system to 9MPa with hydrogen, then raise the temperature to 240°C under stirring, and carry out hydrogenation reaction at the same temperature for 3 hours to obtain an acid value of 145.2mg KOH / g, a softening point of 140°C, and a hue (Haiger color value) of 50. Color aggregated rosin. It was confirmed by GPC that the polymer content in the colorless polymerized rosin was 70.3%, the monomer (hydrogenated product of purified rosin) was 27.7%, and the decomposition product was 2.0%. The colorless polymerized rosin was confirmed by fluorescent X-ray measurement. The amount of sulfur in is 62ppm.

Embodiment 3

[0102] The polymerized rosin was replaced with the polymerized rosin obtained in Example 1, and the polymerized rosin obtained in the same manner as in Example 1 was stored at room temperature in the atmosphere for 2 months, except that the hydrogenation reaction was carried out in the same manner as in Example 2. , to obtain colorless polymerized rosin. The obtained colorless polymerized rosin had an acid value of 144.4 mg KOH / g, a softening point of 138° C., and a hue (Haiger color value) of 80. It was confirmed by GPC that the polymer content in the colorless polymerized rosin was 71.4%, the monomer (hydrogenated product of purified rosin) was 26.4%, and the decomposition product was 2.2%. The colorless polymerized rosin was confirmed by fluorescent X-ray measurement. The amount of sulfur in is 66ppm or less.

[0103] The esterification of embodiment 1

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Abstract

Besides sulfur component of antioxidant, the invention provides polymerized abietate, hydrogenising polymerized abietate with the sulfur component content below 100 ppm, tackifier comprising the polymerized abietate and hydrogenising polymerized abietate, tackifier resin emulision obtained by emulsifying the tackifier, agglutinant / adhesive composition comprising the tackifier; using the drainage agglutinant / adhesive composition comprising the tackifier liquid is able to obtain the polymerized rosin and polymerized abietate which has excellent hue and storage stability (good thermal stability) under heating so as to execute hydrogenation after storing for a long time and is able to hydrogenate (cause the color intensity) the polymerized rosin and polymerized abietate without problem, and obtain the hydrogenising polymerized rosin and polymerized abietate with excellent hue and storage stability, welding paste for lead-free soldering material with excellent hue, and agglutinant / adhesive composition with excellent hue and storage stability and drainage agglutinant / adhesive composition.

Description

technical field [0001] The present invention relates to polymerized rosin, polymerized rosin ester and their hydrogenated products, their production method, flux for soldering, solder paste, tackifying resin, tackifying resin latex, and adhesive / adhesive composition. Background technique [0002] Polymerized rosin is a resin obtained by polymerizing rosins. Since it has a higher softening point than rosin, it is used as it is or stabilized by hydrogenation, and is widely used as a solder flux, a tackifier, and the like. [0003] Since the method of using zinc chloride and sulfuric acid has a high yield, this method has been used as a method for producing polymerized rosin. However, in order to find a higher yield and a simpler method, people have also explored various methods. kind of method. [0004] Patent Document 1 discloses a technique of using, for example, a polymer having a pendant sulfonic acid group as a catalyst. In addition, Patent Document 2 discloses a techni...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09F1/04B23K35/363C09J11/08
Inventor 上垣内学梶田和成
Owner ARAKAWA CHEM IND LTD
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