DOI 10.

1007/s10556-019-00643-4

Chemical and Petroleum Engineering, Vol. 55, Nos. 5-6, September, 2019 (Russian Original Nos. 5-6, May–June, 2019)

RESEARCH, DESIGN, NUMERICAL ANALYSES,

AND OPERATING EXPERIENCE

PROCESSES AND EQUIPMENT OF CHEMICAL AND OIL-AND-GAS

TECHNOLOGIES

DESIGN OF SODIUM CARBOXYMETHYL CELLULOSE PROCESSING HARDWARE

S. A. Svetlov UDC 661.728(045)

The process of obtaining sodium carboxymethyl cellulose from cotton cellulose is discussed. Conceptu-
al and processing-equipment diagrams are presented. The technological process and used equipment are
described.

Keywords: cellulose, carboxymethyl cellulose, preparation, diagram, process, technology, equipment.

Sodium carboxymethyl cellulose (NaCMC) is used in the textile, oil-and-gas, ore beneficiation, construc-
tion, and food industries; in synthetic-detergent, ceramic, and drilling-solution manufacturing; and in flotation
enrichment of ores. NaCMC is also used as a glue base. High-viscosity grades of technical NaCMC are used in
the oil-and-gas industry to stabilize clay suspensions for well drilling [1] and to regulate the filtration and rheo-
logical properties of highly mineralized aqueous drilling solutions at temperatures up to 180°C [2].
Technical NaCMC has regulatory requirements for appearance, as a white to cream-colored fine-grained
fibrous powder; bulk density, up to 800 kg/m 3 ; water mass fraction (for the highest quality product), ≤ 12%;
water solubility, ≥ 98.5%; impurity mass fraction in absolute dry technical product, ≤ 1%; and degree of
polymerization (for various product grades), from 300 to 750. The product quality parameters that determine its
practical applications are the degrees of polymerization and substitution.
The most important property of NaCMC is the ability to prepare low- and high-viscosity aqueous NaCMC
solutions at various temperatures.
The heating time also has a significant effect on the solution viscosity [3].
NaCMC can be prepared by liquid (suspension) and solid-state (heterogeneous) methods. The process
technology and equipment design for NaCMC production by the solid-state method were developed by joint re-
search projects [4, 5].
Technical NaCMC was produced from cotton cellulose (CC) at OAO Polyex using the equipment for cotton
cellulose production that was discussed before [6] and reactor-mixer apparatuses (RMAs) and continuously
stirred mixers (CSMs).
The manufacturing process for technical NaCMC includes the steps of feedstock preparation; drying gas
preparation; basic cellulose preparation (CC mercerization); preparation of the reaction mixture, i.e., a mixture of

Biysk Technological Institute, Branch of I. I. Polzunov Altai State Technical University, Russia; e-mail: sss@bti.secna.ru.

Translated from Khimicheskoe i Neftegazovoe Mashinostroenie, Vol. 55, No. 6, pp. 3−6, June, 2019.

0009-2355/19/0506-0439 © 2019 Springer Science+Business Media, LLC 439

440 S. A. SVETLOV

Fig. 1. Conceptual diagram of sodium carboxymethyl cellulose production.

basic cellulose with sodium monochloroacetate (NaMCA); preparation of moist NaCMC (carboxymethylation);
drying of NaCMC; milling of the product; purification of drying gases; and prepackaging and packaging of the
finished product (Fig. 1).
Mercerization is mainly intended to activate the cellulose in order to increase its reactivity. The process
consists of treating cellulose with aqueous NaOH solution with careful stirring. The NaOH reacts with the cellu-
lose (the process is exothermic) and changes the structure of the cellulose fiber by partially breaking and weak-
ening intermolecular bonds and destroying the cellulose. Mercerization (basic cellulose production) is per-
formed in two steps, i.e., preliminary mixing in a CSM and final mixing in an RMA.
Basic cellulose is a moist, soft, and fibrous material that does not stick to metal surfaces. Wads can be
formed by compressing the moist material.
A solution of cobalt sulfate is added to the RMA to produce low-viscosity NaCMC.
The reaction mixture is prepared in two steps by vigorous stirring of basic cellulose with solid NaMCA
powder. Basic cellulose and the required amount of NaMCA are preliminarily mixed in a CSM and then finally
mixed in an RMA. Carboxymethylation (NaCMC formation) begins upon mixing basic cellulose with NaMCA
and releases a large amount of heat. Hydrolysis of NaMCA to give glycolate (sodium glycolate) and NaCl oc-
curs simultaneously [1]. The hydrolysis rate of NaMCA increases with increasing temperature and amount of
aqueous NaOH in the reaction mixture [7], which decreases the concentration of main compound in the finished
product. Therefore, the mixture is cooled by supplying water at ≤ 15°C to jackets on the CSM, RMA, transport
lines, and hollow rollers to maintain the reaction-mixture temperature at 30–60°C. The water supply is regulated
by a flow meter. The mixture temperature in the RMA is monitored in zones.
Let us examine the NaCMC production process equipment (Fig. 2).

NaCMC Production Process

Highly compressed CC bales (moisture < 8–10%) are raised by an elevator (1) and loaded into the pro-
cessing equipment. The CC is fed by transporter belt 2 into bale opener 3 for wetting the CC with base solution.
Next, the CC is fed into mixer (CSM) 4 where it is preliminary mixed with base solution. The required amount
DESIGN OF SODIUM CARBOXYMETHYL CELLULOSE PROCESSING HARDWARE 441

Fig. 2. Equipment and processing diagram for sodium carboxymethyl cellulose production.

of CC from the opener is continuously fed into the mixer. Simultaneously, the required amount of base solution
(20.5–23.5%) at 15–30°C is added from a storage tank. The base solution is added to the mixer through four
sprayers 5 to improve its distribution in the cellulose. The mixer is equipped with two Z-shaped counter-rotating
stirrers.
The resulting basic cellulose is extruded from the mixer onto horizontal transporter belt 6, from where it en-
ters RMA 7 for final stirring, milling, and neutralization.
The RMA is a horizontal two-belt continuous mixing apparatus with specially designed belts rotating in one
direction. The working volume of the RMA is arbitrarily divided into four zones, each of which has feed inlet
and outlet fittings. The CC and base solution pass through the outlet fittings and are thoroughly mixed. Mix-
er 4, horizontal transporter belt 6, and RMA 7 are water-cooled.
Next, basic cellulose is fed by horizontal and slanted transporter belts 8 and 9 into mixer 10. The obtained
basic cellulose is treated continuously at the outlet of the slanted transporter belt with the required amount of
NaMCA. Basic cellulose and NaMCA are preliminarily mixed in mixer 10 to produce the reaction mixture and
initiate cellulose carboxymethylation. The reaction mixture is extruded from the mixer onto horizontal trans-
porter belt 11 and then into RMA 12, where it is further mixed and milled. Pallets with bags of NaMCA are
raised to the loading area using a mine hoist. The NaMCA is poured from the bags onto a screw conveyer,
where it is milled and then loaded into storage hopper 14. NaMCA is fed onto slanted transporter belt 9 by
feeder 13 from storage hopper 14 (with a spiral stirrer).
The slanted transporter belt, mixer, horizontal transporter belt, and RMA are water-cooled.
The reaction mixture from RMA 12 is fed by horizontal and vertical transporter belts 15 and 16 into finish-
ing tank 17 (steel thermally insulated cylindrical tank with a jacket), which is designed for final carboxymeth-
ylation of the cellulose.
The lower conical part of the finishing tank is equipped with knife blades on a rotating gear. The apparatus
throughput is regulated by the gap between blades.
Carboxymethylation is an exothermic reaction. Therefore, the reaction mixture heats up to 80–120°C as it
moves through the apparatus from above to below. The residence time of the reaction mixture in the finishing
tank (from 20 to 60 min depending on the mixture temperature and grade of obtained NaCMC) is determined by
442 S. A. SVETLOV

the arrangement of knives on the rotating gear. Water vapor is prevented from condensing on the finishing tank
walls by using pump 18 to fill the jacket with hot water from heater 19 supplied by feed tank 20 (or using con-
densate at 90–110°C).
A control panel monitors the temperature in the lower, upper, and middle zones of the finishing tank. Moist
NaCMC is fed from the finishing tank onto transporter belt 21, on which it is further treated with hot air.
Technical NaCMC is dried by developing processes for removing moisture from the moist product using
a flash dryer and a dryer transporter belt. The drying version (Fig. 2) included transporter 21, spreader 22, flash
dryer 23, and fans 24–26.
Moist NaCMC at 80–100°C from the finishing tank is transported by a conveyer belt into the spreader (cen-
trifugal fan) and then into the dryer ejector.
The dryer is equipped with spreaders (active aerodynamic zones for treating moist product), inside of which
fans 25 circulate and rotate moist material to enhance the drying and increase the residence time of product par-
ticles in the dryer to 30–40 sec. The lower part of the dryer has a dust collector with a damper. The steel body
of the flash dryer (pipe and spreader) are thermally insulated from the outside. The heat exchanger (drying
agent, i.e., exhaust gases at 120–180°C) is fed into the dryer by fan 24. A smaller part of the heat exchanger is
fed through transporter belt 21 for preliminary heating of the moist material. The main part of the heat exchang-
er is fed directly into flash dryer 23. The dryer throughput is determined by the flow rates of moist material and
gas and the heat-exchanger temperature. NaCMC dried by heat exchanger is transported into anticyclone 27 to
separate the mixture and precipitate the finished product. Spent heat exchanger is diverted by fan 26 into cy-
clone 28 and scrubber 29 for final purification of the gas stream from suspended particles and dust. Dried prod-
uct is fed from the anticyclone through gate valve 30 into separator 31 and then for prepackaging, packaging,
and storage. The gate valve is a drum (in a cylindrical body) with rubber paddles attached to longitudinal ridges.
The separator is a tank with two unloading belts (rotating against each other) for feeding two streams of dried
NaCMC into bags (set on a balance).
Exhaust gases obtained from burning a propane — butane mixture in gas furnace 32 are used as the heat ex-
changer in the NaCMC drying process. The furnace consists of a heating chamber and a chamber for mixing the
combustion products with air. The upper parts of the chambers are connected by a furnace grate made of refrac-
tory bricks. The combustion chamber contains two gas burners and a valve (in the upper part). Bricks are
placed in a checkerboard pattern in the mixing chamber for better mixing of the exhaust gases and air. The up-
per part of the chamber contains an outlet pipe and natural ventilation valves; the lower part, a gas line. Air is
fed by fan 33 to the combustion chamber burners. Exhaust gases for drying moist NaCMC are supplied by fans
and gas-stream manifolds. The exhaust-gas temperature is regulated by changing the amount of air fed into the
mixing chamber.
The working base solution is prepared and dispensed using volumetric equipment and pumps.
NaOH solution from a warehouse is pumped into the dispensing tank where it is diluted with condensate or
filtered water to a concentration of 20.5–23.5%.
The prepared solution is fed by pump 34 from dispensing tank 35 into supply tank 36 in which it is heated
as necessary to 18–20°C by condensate passing through the pipe (in the lower part of the tank). Base solution
passes from the supply tank through filter 37 and pump-dispenser 38 through sprayer 5 into the cellulose stream
entering mixer 4 for mixing base and milled cellulose. The solution supply lines to the sprayers are fitted with
heat exchanger 39 to heat the base solution using condensate (in winter) or to cool it with water (in summer) to
15–30°C. The pipe is purged with compressed air from tank 40.
Dusty air from storage hopper 14 is fed by a fan into cyclone 41 for purification. Purified air from the cy-
clone is exhausted to the atmosphere. Dust enters the storage hopper, from which it is periodically removed for
further recycling.
DESIGN OF SODIUM CARBOXYMETHYL CELLULOSE PROCESSING HARDWARE 443

Packaging of NaCMC uses balance 42 and 4- or 5-ply paper bags (the ends of the bags are sewn closed on
sewing machine 43) that are transported to the finished product warehouse by an electric or conventional fork-
lift 44. NaCMC is stored in dry sealed rooms without intrusion of moisture and acidic vapor.

CONCLUSION

Features of the process for solid-state preparation of technical NaCMC from CC were found by the research
and operation of industrial equipment. The equipment in certain processing operations could be improved and
updated to increase the process throughput, reduce energy losses, and improve the quality of the finished prod-
uct. Results of scientific research and design work were used to develop machines and apparatuses for NaCMC
production technology.

REFERENCES

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241-253 (1959).
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