CN1174202A

CN1174202A - Ethoxyl cellulose producing process from plant cotton

Info

Publication number: CN1174202A
Application number: CN 96115530
Authority: CN
Inventors: 鞠馥阳; 刘伟
Original assignee: Individual
Current assignee: Individual
Priority date: 1996-08-15
Filing date: 1996-08-15
Publication date: 1998-02-25

Abstract

Through the technological process of dip lye, squeezing, tearing, etherification alcohol washing, tumble drying, stoving and crushing, plant cotton as raw material is made into hydroxyethyl cellulose. The present invention uses cheap material to produce hydroxyethyl cellulose product through easy-to-control technological process.

Description

Manufacture the method for Natvosol with plant cotton

The present invention be a kind of be the method that raw material is manufactured Natvosol with the plant cotton.

Natvosol is an oil, ore dressing, weaving, printing and dyeing, medicine, chemical industry, papermaking, the industrial raw material that industries such as coating are important, be in great demand, and the method for traditional production Natvosol, no matter adopt vapour phase processes or liquid phase method, used raw material all is a refined cotton linter, develop rapidly along with industry, the growth year by year of the city size expansion and the size of population, cultivated area is reduced year by year, the cultivated area of cotton is also fewer and feweri, be difficult to satisfy with the linters production demand of the Mierocrystalline cellulose series product that is raw material, the utmost point waits to develop a kind of new raw material that can the replace cotton short flannel.

The objective of the invention is to, provide a kind of raw material to be easy to get, production technique is easy, and what cost of manufacture was low manufactures the method for Natvosol with plant cotton.

Following mode can realize the present invention:

To be plant cotton wash → dry → dry → pulverize through caustic dip → squeeze → tear up → etherificate → alcohol the manufacture craft flow process, it is as follows that step is made in its gymnastics: after the first step is measured plant cotton, dropping into concentration is the caustic soda solution of 18.3 ° of Be ', and caustic dip took out after 30-40 minute; Second step was sent into squeezing machine to the caustic dip plant cotton that takes out, and press ratio is 1: 3.2; The alkali fiber that the 3rd step will reach press ratio tears up; The 4th step was dropped into the etherificate still with the alkali fiber that tears up, and vacuumized after the sealing, and vacuum tightness reaches 760; The 5th step charged into nitrogen in the oxyethane bottle, get rid of the air in it; The 6th step was aimed at central siphon in the etherificate still to mouth before the oxyethane bottle, by the nitrogen at rear portion oxyethane was pushed the etherificate still, and its amount is that per 1 kilogram plant cotton charges into 1.3 kilograms oxyethane; The 7th step sprayed brine refrigeration immediately when temperature of reaction rises to 24 ℃, make the interior top temperature of etherificate be no more than 34 ℃, when still top temperature indicator is indicated to 22 ℃, stopped to spray salt solution, discharging after static again 3-5 minute; The 8th step filled whole etherificate material inputs in the washing still of industrial alcohol, and submergence is stirred, and drops into acetic acid after 20 minutes, and 0.6 kilogram of acetic acid of metering per kilogram plant cotton input neutralizes when feeding intake, and makes pH value reach 6; Plant cotton after the 9th step was washed alcohol carries out centrifuge dripping; The tenth step was washed the etherificate fiber secondary alcohol that dries, after 15 minutes, with phenolphthalein reagent examination inspection, if phenolphthalein is light red, drench acetic acid more in a small amount, when the phenolphthalein redfree occurs, the fiber that secondary alcohol is washed is centrifuge dripping again, and fiber dries when an ethanol does not go out yet, discharging; The 11 step was dried into the cloudlet shape with the fiber that dries; The fiber of the 12 step oven dry is ground into 100 purpose powder, is packaged into finished product.

Plant cotton is the same with the purified linters, has the Mierocrystalline cellulose more than 94%, the composition of all the other less thaies 5% is a hemicellulose, 1% composition is an xylogen, replaces linters to make Natvosol with plant cotton, and raw material is easy to get, cost is low, easy control of process conditions, required equipment is few, the requirement that is up to state standards fully of finished product Natvosol.

Embodiment:

With 100 kilograms of plant cottons is example, the alkali that drops on the squeezing machine soaks in the case, prepare the caustic soda solution that concentration is 18.3 ° of Be ' in the case in advance, soak after 40 minutes and to start squeezing machine and squeeze, press ratio is 1: 3.2, the alkali fiber that will reach press ratio tears up, again the alkali fiber that tears up is dropped into the etherificate still, vacuumize after the sealing, vacuum tightness this 760, in the oxyethane bottle, charge into nitrogen, to discharge the air in it, mouth before the bottle is aimed at central siphon in the etherificate still, start the valve on the still, nitrogen by the bottle rear portion pushes the etherificate still to oxyethane, 100 kilograms plant cotton charges into 130 kilograms oxyethane, this is thermopositive reaction, when temperature rises to 24 ℃, open brine valve spray refrigeration immediately, make that the temperature of reaction of etherificate still is the highest to be no more than 34 ℃, approximately through 2.5 hours, when etherificate still top temperature indicator slides to 22 ℃ down gradually, stop to spray salt solution, stop discharging after 3 minutes again, then whole etherificate fibers is dropped in the washing still of 300 kilograms of industrial alcohols, carrying out alcohol embathes, be as the criterion with ethanol submergence fiber, open the agitator of washing still, stir and drop into 60 kilograms of acetic acid after 20 minutes, neutralize, make pH value this 6, fiber after alcohol washed is put into whizzer and is dried, the impure ethanol that throws away enters in the ground cylinder from the upflow tube on the whizzer and collects, and it is pure to send the pure still steaming of steaming to vacuum primingpump again, when temperature reaches 78 ℃, the ethanol vaporization, steam after filtration, purify, condensation, reclaim, multiplexingly wash the etherificate fiber, save the input amount of industrial alcohol in alcohol, next step carries out secondary alcohol with the etherificate fiber that dries and washes, soak after 15 minutes, with phenolphthalein reagent examination inspection, if phenolphthalein is light red, in the washing still, drench acetic acid more in a small amount, when the phenolphthalein redfree occurs, take out fiber, centrifuge dripping, still reclaiming the pure back of ethanol steaming reclaims multiplexing, get rid of when an ethanol does not go out yet, discharging divides and puts in the baking tray, slow baking is 6-7 hour under 60-75 ℃ of temperature, drying, fiber become the cloudlet shape, and pulverized fiber is 100 orders then, getting product promptly is Natvosol, through the packing warehouse-in.

Claims

1. manufacture the method for Natvosol with plant cotton for one kind, step is, the first step with the plant cotton metering after, dropping into concentration is the caustic soda solution of 18.3Be ', caustic dip took out after 30-40 minute; Second step was sent into squeezing machine to the caustic dip plant cotton that takes out, and press ratio is 1: 3.2; The alkali fiber that the 3rd step will reach press ratio tears up; The 4th step was dropped into the etherificate still with the alkali fiber that tears up, and vacuumized after the sealing, and vacuum tightness reaches 760; The 5th step charged into nitrogen in the oxyethane bottle, get rid of the air in it; The 6th step was aimed at central siphon in the etherificate still to mouth before the oxyethane bottle, by the nitrogen at rear portion oxyethane was pushed the etherificate still, and its amount is that per 1 kilogram plant cotton charges into 1.3 kilograms oxyethane; The 7th step sprayed brine refrigeration immediately when temperature of reaction rises to 24 ℃, make the interior top temperature of etherificate still be no more than 34 ℃, when still top temperature indicator is indicated to 22 ℃, stopped to spray salt solution, discharging after static again 3-5 minute; The 8th step filled whole etherificate material inputs in the washing still of industrial alcohol, and submergence is stirred, and drops into acetic acid after 20 minutes, and 0.6 kilogram of acetic acid of metering per kilogram plant cotton input neutralizes when feeding intake, and makes pH value reach 6; Plant cotton after the 9th step was washed alcohol carries out centrifuge dripping; The tenth step was washed the etherificate fiber secondary alcohol that dries, after 15 minutes, with phenolphthalein reagent examination inspection, if phenolphthalein is light red, drench acetic acid more in a small amount, when the phenolphthalein redfree occurs, the fiber that secondary alcohol is washed is centrifuge dripping again, and fiber dries when an ethanol does not go out yet, discharging; The 11 step was dried into the cloudlet shape with the fiber that dries; The fiber of the 12 step oven dry is ground into 100 purpose powder, is packaged into finished product.

2. method according to claim 1 is characterized in that: the 9th step, the tenth step are sent into the pure still of steaming and steam pure after getting rid of the ethanol collection that contains impurity such as buck of usefulness when drying, in the time of these 78 ℃, ethanol becomes steam, after filtration, purify, be condensed into purified ethanol, is used further to the washing to the etherificate fiber.