CN1168912A

CN1168912A - Temp. phase transformation art for all-free dispersion rosin size

Info

Publication number: CN1168912A
Application number: CN 96107678
Authority: CN
Inventors: 魏震宇; 许东生
Original assignee: ANHUI CHEMICAL ENGINEERING INST
Current assignee: ANHUI CHEMICAL ENGINEERING INST
Priority date: 1996-06-14
Filing date: 1996-06-14
Publication date: 1997-12-31

Abstract

Add prepared emulsifying agent solution to melted rosin under constant stirring, continue adding water until oil-watrer ratio is 1:0.8-1.2, and mix to obtain W\O emulsion. Then lower the temp. and convert the system to O\W type completely free and dispersed rosin glue. The whole technology is fulfilled in s kettle, the operation is simple, reaction is even and easy to control and the quality is stable. The product produced by the invented technology is milky white in appearance, its solid content greater than or equal to 50%, in which the rosin eontent is up to 40%, pH valve 5-6, viscosity (25deg. C) smaller than or equal to 25 CP.

Description

Complete free dispersion rosin size temperature phase inversion novel process

The present invention relates to the mutual dispersive technology of a kind of profit, specifically the free full dispersion rosin size temperature phase inversion novel process in a place.

Saponification rosin is sizing agent traditional in the paper industry.Still is using in domestic most of paper mills at present.This sizing agent writing paper per ton will consume the rosin more than 15 kilograms, not only wastes resource, and the finished paper quality is low, also the fugitive sizing phenomenon can take place in summer.

The U.S., states such as Japan have just begun the research and development of dispersion rosin size as far back as the seventies, and up-to-date research direction remains from molecular structure rosin is given modification, makes the anionic dispersion rosin size.Domestic each related research units begins rosin sizing agent is researched and developed from the seventies, successively works out fortified rosin soap powder and sizepine P, but is inconvenient to be difficult to promote because of using.Research and develop dispersion rosin size in succession to late nineteen eighties, but its emulsifying stability is especially also unsatisfactory in summer, promotes the use of to be restricted.

Its essence of the preparation process of dispersion rosin size is exactly the emulsion process that rosin is distributed to equably the stable oil-in-water-type of formation in the water.Rosin is solid and water insoluble, even viscosity is also very big when being heated to 100 ℃ (boiling point of water).So solve scattering problem, be suitable for beyond the rosin emulsive emulsifying agent except rosin being carried out modification (known method is with the addition of cis-butenedioic anhydride diene, increases the rosiny acid number, improves wetting ability) and selection, its technology also directly relates to the quality of product.This technology relates to the phase transition problem, because product also will be converted the water dilution when applying glue, water is external phase, oil (rosin and modified rosin) is disperse phase, be emulsion oil-in-water, and be water-in-oil-type (W/O) when system begins in technological process, must change oil-in-water-type (O/W) into.In the prior art, the phase inversion that has with the change of system component, and the present invention be system with the change of temperature phase inversion.

According to reported in literature, the technology for preparing this glue has three kinds, the one, solvent method, with organic solvent rosin is dissolved earlier, then with rosin solution with the emulsifier aqueous solution mixing and emulsifying, last vacuum desolventizing reclaims organic solvent, can make the stable emulsion of solid content 35～40%, this method of Japanese waste river chemistry of forest product Co., Ltd..The 2nd, high temperature and high pressure method, with fusing and be warmed up to 160～190 ℃ rosin and mix by the high pressure homogenisers forced emulsification with the emulsifier aqueous solution that is preheating to 80～90 ℃, be cooled to below 38 ℃ then rapidly, can make the stable emulsion of solid content 35～40%, U.S. Monsanto Company promptly uses this method.In view of solvent method need use and reclaim solvent, make originally simple process complications, and pollution is arranged; The required high pressure homogenisers of high temperature and high pressure method costs an arm and a leg, facility investment is big, operation also acquires a certain degree of difficulty, so having developed a kind of normal pressure, more domestic professional institutes add water anti-phase method, at first the emulsifier aqueous solution input is dissolved in the mixed rosin under the state and make the w/o type emulsion, adding phase inversion water (hot water) fast under high-speed stirring (1600 change above/minute) condition changes the component of system then, phase reversal of emulsion becomes the O/W type, and last cooling rapidly promptly gets dispersion rosin size.This method technology is simple, and operational safety, but require a high-speed mixing equipment adds water and wants fast, and cooling is wanted rapidly, so produce waywardly, quality product is stable inadequately, and heat-storage stability is also not ideal enough, can not satisfy the needs of paper industry.

The objective of the invention is to provide in the preparation process for dispersion rosin size a kind of new phase transfer process, smooth operation not only, control, and the quality of product easily improves comprehensively, especially has excellent heat-storage stability.

The present invention is transformed into O/W type with system by w/o type by variation of temperature, concrete technology is as follows: fusing at first heats up rosin, under agitation condition, drop into the emulsifier aqueous solution for preparing then and make the w/o type emulsion, continue to add water, up to water oil ratio to 1: till 0.8～1.2, and holding temperature is between 100～120 ℃, under this temperature, oil is still external phase in the system, and water is disperse phase, is the w/o type emulsion.Water adds and the back that stirs lowers the temperature, and along with decrease of temperature, the rerum natura of rosin and water changes thereupon, thereby realizes being transformed into the O/W type by w/o type.The temperature of phase inversion point is different and different with emulsifying agent, can be under 60～95 ℃ of differing tempss phase inversion.

The chemical industry equipment that this technology is general just can satisfy processing requirement, and whole process is finished in a still, and is simple to operate, reacting balance, control easily, favorable reproducibility, steady quality.Complete free its outward appearance of dispersion rosin size with this explained hereafter is the emulsion of milky white colour band blue streak, solid content 〉=50%, and wherein rosin content is up to more than 40%; PH value is 5～6; Viscosity (25 ℃) is≤25CP; 10 days (with storing 1 year equivalence naturally) no changes of heat storage (54 ℃), actual heat-storage still can be used in 1 month.Because the product Heat stability is good, so still normally applying glue in summer, the rosiny consumption reduces greatly.With the product of this processes, every index all reaches domestic state-of-the-art level, and its heat-storage stability occupies the top standard.

Embodiment:

1, gets 333g and 111g modified rosin and drop in the beaker heat fused together; Get 150gWSH-18 emulsifier aqueous solution (active constituent content is 30%), under stirring (60 rev/mins), drop in the rosin, continue to add water to system and reach 1000g, stir, and holding temperature is at 100～120 ℃.At this temperature lower body is the w/o type emulsion.Close thermal source, just obtain the free full dispersion rosin size of O/W type when under agitation being cooled to 90 ℃.Appearance milky white has blue streak.

2, get 333g and 111g modified rosin and drop in the beaker heat fused together; Get 180gWSH-20 emulsifier aqueous solution (active constituent content is 25%), under stirring (60 rev/mins), drop in the rosin, continue to add water to system and reach 1100g, stir, and holding temperature is at 100～120 ℃.Close thermal source, just obtain the complete free dispersion rosin size of O/W type oyster white, band blue streak when under agitation being cooled to 75 ℃.

3, get 333g and 111g modified rosin and drop in the beaker heat fused together; Get 225gWSH-21 emulsifier aqueous solution (active constituent content is 20%), under stirring (60 rev/mins), drop in the rosin, continue to add water to system and reach 900g, stir, and holding temperature is at 100～120 ℃.Close thermal source, just obtain the complete free dispersion rosin size of O/W type oyster white, band blue streak when under agitation being cooled to 60 ℃.

Above process scalable 1000 times at 1M ³Carry out in the reactor.

Claims

1, a kind of complete free dispersion rosin size temperature phase inversion novel process, by rosin, emulsifying agent and the water processing earlier of fusing obtain the w/o type emulsion again phase inversion become O/W type emulsion, it is characterized in that: realize the phase inversion of system by variation of temperature, concrete technology is as follows:

(1), in the mixed rosin with the fusing of the emulsifier aqueous solution input for preparing under agitation condition, continuing to add water to water oil ratio is 1: 0.8～1.2, and holding temperature obtains the w/o type emulsion at 100～120 ℃,

(2), the back that stirs lowers the temperature under 100～120 ℃ of temperature, phase inversion obtains the free full dispersion rosin size of O/W type in the time of 60～90 ℃.