Method for determining the degree of completion and pulp yield

• US 4,540,468 A
• Filed: 09/26/1983
• Issued: 09/10/1985
• Est. Priority Date: 09/26/1983
• Status: Expired due to Fees

• Current Assignee: The University Of Maine
• Original Assignee: Board of Trustees of The University of Maine
• Inventors: Genco, Joseph M., Hassler, John C.
• Primary Examiner(s): Alvo, Steve
• Application Number:
  US06/535,922
• Time in Patent Office: 715 Days
• Field of Search: 162/49, 162/238, 162/263, 162/DIG. 10, 162/61, 162/62, 436/146
• US Class Current: 162/49
• CPC Class Codes: D21C 3/228 Automation of the pulping processes
• CPC Class Codes: Y10T 436/235 In an aqueous solution [e.g., TOC, etc.]

Abstract

A method is described for monitoring and determining the degree of completion, pulp yield, and residual lignin content in a pulping or delignification reaction. The system provides an on-line, real time, closed loop process control system for the reaction of a known quantity of wood in process liquor. The desired pulp yield is achieved by sampling the liquor during the reaction; determining the total organic carbon content of the sampled liquor; and calculating the degree of completion of the reaction and pulp yield from the process liquor total organic carbon content determination using an appropriate mathematical model. The mathematical model is based upon conservation of carbon mass in the wood or pulp and liquor during the reaction, and includes a conservation of mass equation in which the total organic carbon in the sampled liquor substantially equals the total carbon in the starting quantity of wood or pulp less the total carbon in pulp wood residue at the time of sampling the liquor. Variations of the basic system and method are described.

Claims

1. In a method for monitoring and determining the degree of completion and pulp yield of a pulping or delignification reaction for a known quantity of starting wood or pulp of known carbon content immersed and reacting in a process liquor of known starting carbon content at a known liquor to wood or pulp ratio the improvement comprising:

sampling the liquor during the reaction;

measuring the total organic carbon content of the sampled liquor during the reaction;

calculating the degree of completion of the reaction and pulp yield from the process liquor total organic carbon content measurement using a conservation of carbon mass mathematical model based upon conservation of carbon mass in the wood or pulp and liquor during the reaction, said mathematical model including a conservation of mass equation in which the total organic content in the sampled liquor substantially equals the total carbon content in the starting quantity of wood or pulp less the total carbon content of wood residue at the time of sampling the black liquor, said mathematical mode providing the calculation of the degree of completion and pulp yield based upon the sampled liquor total organic carbon measurement without requiring sampling of the wood or pulp residue of the pulping or delignification reaction;

controlling the reaction in real time according to the calculated degree of completion and pulp yield of the reaction;

and terminating the reaction when the reaction reaches the desired degree of completion and pulp yield calculated by the conservation of carbon mass mathematical model applied to the sampled liquor total organic carbon measurement.

2. The method of claim 1 wherein the step of measuring the total organic carbon content of the sampled liquor comprises measuring and determining the total carbon content of the sampled liquor.

3. The method of claim 2 wherein the step of measuring and measuring the total carbon content comprises combusting the sampled liquor and measuring the quantity of carbon dioxide.

4. The method of claim 3 wherein the step of measuring the quantity of carbon dioxide comprises measuring the quantity of carbon dioxide with an infrared analyzer.

5. The method of claim 3 wherein the step of measuring the total carbon dioxide comprises measuring the quantity of carbon dioxide gravimetrically.

6. The method of claim 2 wherein the step of measuring the total carbon content comprises measuring and determining the quantity of radioactive carbon isotopes present in the liquor sample and inferring the total carbon from the measured fractional radioactive carbon isotopes.

7. The method of claim 1 wherein the step of sampling the liquor during the pulping reaction comprises continuously sampling the liquor.

8. The method of claim 1 wherein the step of determining the total organic carbon content of the sampled liquor comprises determining the total carbon content of the sampled liquor, determining the total inorganic carbon content of the sampled liquor, and subtracting the inorganic carbon content from total carbon content to give the total organic carbon content.

9. The method of claim 8 wherein the step of measuring the total carbon content comprises combusting a first portion of the liquor sample and measuring the total carbon from the carbon dioxide generated by the combustion of the liquor sample;

acidifying a second portion of the liquor sample and heating the acidified sample to drive off the inorganic carbon as carbon dioxide and determining the total inorganic carbon by measuring said carbon dioxide; and

subtracting the total inorganic carbon from the total carbon to give the total organic carbon content of the liquor.

10. The method of claim 1 wherein the step of controlling the reaction according to the calculated degree of completion and yield comprises controlling the time duration of the reaction.

11. The method of claim 1 wherein the step of controlling the reaction comprises controlling the temperature of the reaction.

12. The method of claim 1 wherein the step of controlling the reaction comprises controlling the ratio by weight of the liquor to wood or pulp.

13. The method of claim 1 further comprising the step of calculating the Kappa number corresponding to the lignin content of the pulp from the total organic carbon content measurement using conservation of carbon mass mathematical model, said model substantially approximating empirically established linear relationship between process liquor total organic carbon content and Kappa number.

14. The method of claim 1 further comprising the step of calculating the heat value of the liquor from the total organic carbon content measurement using a conservation of carbon mass mathematical model substantially approximating the empirically established linear relationship between process liquor total organic carbon content and heat value of the liquor.

15. The method of claim 1 further comprising the step of correcting the H-factor corresponding to the further reaction time to desired degree of completion and pulp yield from the total organic carbon content measurement using said conservation of carbon mass mathematical model.

16. The method of claim 1 wherein the reaction is a primary delignification or pulping reaction and wherein said liquor is a black liquor.

17. The method of claim 1 wherein the reaction is a secondary delignification or bleaching reaction and wherein said liquor is a bleaching liquor.

18. In a method for monitoring and determining the degree of completion and pulp yield of a pulping or delignification reaction for a known quantity of starting wood of identified characteristics immersed and digesting in a known quantity of black liquor at a known black liquor to wood ratio, the improvement comprising:

sampling the starting black liquor and measuring the dead load organic carbon content of the starting black liquor;

determining the total carbon content in the known quantity of starting wood;

sampling the black liquor during the pulping reaction;

measuring the total organic carbon content of the sampled black liquor during the reaction;

calculating the degree of completion of the pulping reaction and pulp yield from the sampled black liquor total organic carbon content measurement using a conservation of carbon mass mathematical model based upon conservation of carbon mass in the wood and black liquor during the reaction, said mathematical model including a conservation of mass equation in which the total organic carbon content in the sampled black liquor less any dead load organic carbon content measured in the starting black liquor substantially equals the total carbon content in the starting quantity of wood less the total carbon content in the of wood residue at the time of sampling the black liquor, said mathematical model providing the calculation of degree of completion and pulp yield based upon the sampled black liquor total organic carbon measurement without requiring sampling of the wood or pulp residue of the pulping or delignification reaction;

controlling the pulping reaction in real time according to the calculated degree of completion and pulp yield of the pulping reaction;

and terminating the pulping reaction when the reaction reaches the desired degree of completion and pulp yield predicted by the mathematical model based upon the sampled black liquor total organic carbon content measurement.

19. The method of claim 18 wherein the step of controlling the pulping reaction in real time comprises controlling the duration, temperature, or black liquor to wood ratio of the pulping reaction.